Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806048914/ng2128sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806048914/ng2128Isup2.hkl |
CCDC reference: 633927
Key indicators
- Single-crystal X-ray study
- T = 193 K
- Mean (C-C) = 0.004 Å
- R factor = 0.030
- wR factor = 0.070
- Data-to-parameter ratio = 15.3
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.62 mm PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 4 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.63 Ratio PLAT245_ALERT_2_C U(iso) H18A Smaller than U(eq) C18 by ... 0.03 AngSq PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C16
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 26.40 From the CIF: _reflns_number_total 2791 Count of symmetry unique reflns 1569 Completeness (_total/calc) 177.88% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1222 Fraction of Friedel pairs measured 0.779 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1999); cell refinement: SMART; data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SIR2004 (Burla et al., 2005); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Co(C24H40BN6)Cl] | F(000) = 1100 |
Mr = 517.81 | Dx = 1.229 Mg m−3 |
Orthorhombic, Ama2 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: A 2 -2a | Cell parameters from 3253 reflections |
a = 16.429 (2) Å | θ = 2.3–26.0° |
b = 16.035 (2) Å | µ = 0.73 mm−1 |
c = 10.6255 (14) Å | T = 193 K |
V = 2799.1 (6) Å3 | Plate, blue |
Z = 4 | 0.62 × 0.4 × 0.09 mm |
Bruker SMART CCD area-detector diffractometer | 2594 reflections with I > 2σ(I) |
φ and ω scans | Rint = 0.032 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | θmax = 26.4°, θmin = 2.3° |
Tmin = 0.660, Tmax = 0.937 | h = −14→20 |
6423 measured reflections | k = −20→19 |
2791 independent reflections | l = −10→13 |
Refinement on F2 | H atoms treated by a mixture of independent and constrained refinement |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0311P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.030 | (Δ/σ)max < 0.001 |
wR(F2) = 0.07 | Δρmax = 0.29 e Å−3 |
S = 1.05 | Δρmin = −0.21 e Å−3 |
2791 reflections | Absolute structure: Flack (1983), 1228 Friedel pairs |
183 parameters | Absolute structure parameter: 0.004 (14) |
1 restraint |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
C13 | 0.25 | 0.1247 (2) | 0.2499 (3) | 0.0285 (7) | |
C14 | 0.25 | 0.1628 (2) | 0.1328 (3) | 0.0333 (8) | |
H14 | 0.25 | 0.1356 | 0.0533 | 0.04* | |
C15 | 0.25 | 0.2471 (2) | 0.1536 (3) | 0.0298 (7) | |
C16 | 0.25 | 0.3178 (3) | 0.0615 (3) | 0.0431 (11) | |
C17 | 0.25 | 0.0319 (2) | 0.2832 (4) | 0.0373 (8) | |
C18 | 0.25 | −0.0176 (3) | 0.1599 (5) | 0.0623 (13) | |
C19 | 0.32656 (18) | 0.01066 (15) | 0.3567 (3) | 0.0493 (7) | |
H19A | 0.3746 | 0.0247 | 0.3061 | 0.059* | |
H19B | 0.327 | −0.0491 | 0.3761 | 0.059* | |
H19C | 0.3275 | 0.0427 | 0.4352 | 0.059* | |
C23 | 0.08693 (13) | 0.30655 (13) | 0.5822 (2) | 0.0244 (5) | |
C24 | 0.05763 (11) | 0.38008 (12) | 0.5287 (3) | 0.0282 (4) | |
H24 | 0.0087 | 0.4083 | 0.5503 | 0.034* | |
C25 | 0.11301 (12) | 0.40389 (13) | 0.4388 (2) | 0.0238 (4) | |
C26 | 0.11477 (14) | 0.47947 (14) | 0.3568 (2) | 0.0329 (5) | |
H26A | 0.163 | 0.4776 | 0.3027 | 0.039* | 0.5 |
H26B | 0.1167 | 0.5296 | 0.4094 | 0.039* | 0.5 |
H26C | 0.0657 | 0.4808 | 0.3044 | 0.039* | 0.5 |
H26D | 0.0673 | 0.5144 | 0.375 | 0.039* | 0.5 |
H26E | 0.1136 | 0.4624 | 0.2682 | 0.039* | 0.5 |
H26F | 0.1646 | 0.5112 | 0.3733 | 0.039* | 0.5 |
C27 | 0.04844 (13) | 0.25419 (15) | 0.6852 (2) | 0.0301 (5) | |
C28 | −0.03048 (17) | 0.29516 (19) | 0.7285 (3) | 0.0525 (8) | |
H28A | −0.0551 | 0.2615 | 0.7954 | 0.063* | |
H28B | −0.0682 | 0.2991 | 0.6574 | 0.063* | |
H28C | −0.0188 | 0.3512 | 0.7607 | 0.063* | |
C29 | 0.10641 (15) | 0.24910 (17) | 0.7983 (2) | 0.0393 (6) | |
H29A | 0.0815 | 0.2152 | 0.8646 | 0.047* | |
H29B | 0.1169 | 0.3054 | 0.8305 | 0.047* | |
H29C | 0.1578 | 0.2235 | 0.772 | 0.047* | |
C30 | 0.02961 (17) | 0.16691 (17) | 0.6349 (3) | 0.0435 (7) | |
H30A | 0.0052 | 0.1332 | 0.7019 | 0.052* | |
H30B | 0.0801 | 0.1404 | 0.6063 | 0.052* | |
H30C | −0.0085 | 0.1712 | 0.5642 | 0.052* | |
B | 0.25 | 0.3422 (2) | 0.3546 (3) | 0.0223 (7) | |
N11 | 0.25 | 0.25942 (16) | 0.2785 (2) | 0.0240 (5) | |
N12 | 0.25 | 0.18371 (16) | 0.3391 (2) | 0.0260 (6) | |
N21 | 0.17306 (10) | 0.34638 (10) | 0.43716 (16) | 0.0202 (4) | |
N22 | 0.15729 (9) | 0.28569 (9) | 0.5266 (2) | 0.0213 (3) | |
Cl | 0.25 | 0.09500 (5) | 0.65949 (9) | 0.0421 (2) | |
Co | 0.25 | 0.20140 (2) | 0.52764 (3) | 0.02200 (11) | |
H1 | 0.25 | 0.3939 (19) | 0.292 (3) | 0.026 (8)* | |
H18A | 0.25 | −0.071 (3) | 0.177 (4) | 0.037 (10)* | |
H18B | 0.302 (2) | −0.002 (2) | 0.107 (3) | 0.078 (11)* | |
H16A | 0.296 (2) | 0.351 (2) | 0.079 (3) | 0.076 (11)* | |
H16B | 0.25 | 0.296 (2) | −0.017 (4) | 0.052 (14)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C13 | 0.0226 (16) | 0.0303 (17) | 0.0326 (17) | 0 | 0 | −0.0095 (13) |
C14 | 0.0317 (18) | 0.040 (2) | 0.0278 (18) | 0 | 0 | −0.0108 (14) |
C15 | 0.0238 (17) | 0.043 (2) | 0.0224 (15) | 0 | 0 | −0.0042 (15) |
C16 | 0.056 (3) | 0.056 (3) | 0.0170 (19) | 0 | 0 | 0.0042 (15) |
C17 | 0.043 (2) | 0.0258 (18) | 0.0427 (19) | 0 | 0 | −0.0125 (16) |
C18 | 0.086 (4) | 0.033 (2) | 0.068 (3) | 0 | 0 | −0.026 (2) |
C19 | 0.0482 (17) | 0.0295 (14) | 0.0701 (19) | 0.0063 (12) | −0.0001 (14) | −0.0032 (12) |
C23 | 0.0194 (11) | 0.0286 (12) | 0.0252 (10) | −0.0021 (9) | −0.0011 (9) | 0.0006 (8) |
C24 | 0.0200 (9) | 0.0301 (10) | 0.0345 (10) | 0.0038 (8) | 0.0051 (12) | 0.0009 (13) |
C25 | 0.0193 (10) | 0.0239 (11) | 0.0280 (10) | 0.0002 (8) | −0.0017 (9) | 0.0031 (9) |
C26 | 0.0249 (12) | 0.0309 (13) | 0.0428 (14) | 0.0048 (10) | 0.0001 (10) | 0.0111 (10) |
C27 | 0.0224 (12) | 0.0375 (13) | 0.0305 (13) | −0.0025 (10) | 0.0044 (10) | 0.0094 (9) |
C28 | 0.0342 (15) | 0.067 (2) | 0.0557 (19) | 0.0050 (13) | 0.0201 (13) | 0.0205 (15) |
C29 | 0.0428 (14) | 0.0511 (17) | 0.0241 (11) | −0.0042 (12) | 0.0011 (11) | 0.0051 (11) |
C30 | 0.0404 (16) | 0.0437 (15) | 0.0464 (17) | −0.0159 (12) | 0.0012 (12) | 0.0102 (12) |
B | 0.0217 (17) | 0.0225 (18) | 0.0228 (17) | 0 | 0 | 0.0052 (14) |
N11 | 0.0258 (13) | 0.0275 (14) | 0.0186 (12) | 0 | 0 | 0.0034 (10) |
N12 | 0.0308 (14) | 0.0212 (13) | 0.0261 (14) | 0 | 0 | −0.0004 (10) |
N21 | 0.0202 (9) | 0.0213 (9) | 0.0192 (8) | −0.0004 (7) | −0.0015 (7) | 0.0032 (7) |
N22 | 0.0218 (7) | 0.0214 (8) | 0.0206 (7) | −0.0017 (6) | −0.0002 (11) | 0.0041 (9) |
Cl | 0.0441 (5) | 0.0355 (4) | 0.0466 (5) | 0 | 0 | 0.0216 (4) |
Co | 0.02350 (19) | 0.01983 (19) | 0.02269 (19) | 0 | 0 | 0.0043 (2) |
Co—Cl | 2.2076 (9) | C19—H19C | 0.98 |
Co—N12 | 2.023 (3) | N22—C23 | 1.341 (3) |
Co—N22 | 2.0364 (15) | C23—C24 | 1.395 (3) |
Co—N22i | 2.0364 (15) | C23—C27 | 1.517 (3) |
N11—N12 | 1.375 (3) | C24—C25 | 1.373 (3) |
N21—N22 | 1.385 (3) | C24—H24 | 0.95 |
B—N11 | 1.554 (4) | C25—N21 | 1.351 (3) |
B—N21 | 1.540 (2) | C25—C26 | 1.493 (3) |
B—N21i | 1.540 (2) | C26—H26A | 0.98 |
B—H1 | 1.06 (3) | C26—H26B | 0.98 |
N12—C13 | 1.340 (4) | C26—H26C | 0.98 |
C13—C14 | 1.386 (5) | C26—H26D | 0.98 |
C13—C17 | 1.530 (5) | C26—H26E | 0.98 |
C14—C15 | 1.370 (5) | C26—H26F | 0.98 |
C14—H14 | 0.95 | C27—C28 | 1.525 (3) |
C15—N11 | 1.342 (4) | C27—C30 | 1.530 (4) |
C15—C16 | 1.497 (5) | C27—C29 | 1.536 (3) |
C16—H16A | 0.95 (3) | C28—H28A | 0.98 |
C16—H16B | 0.91 (4) | C28—H28B | 0.98 |
C17—C19 | 1.519 (4) | C28—H28C | 0.98 |
C17—C19i | 1.519 (4) | C29—H29A | 0.98 |
C17—C18 | 1.531 (6) | C29—H29B | 0.98 |
C18—H18A | 0.87 (4) | C29—H29C | 0.98 |
C18—H18B | 1.05 (3) | C30—H30A | 0.98 |
C19—H19A | 0.98 | C30—H30B | 0.98 |
C19—H19B | 0.98 | C30—H30C | 0.98 |
N11—N12—Co | 109.91 (18) | C25—C26—H26A | 109.5 |
N21—N22—Co | 109.28 (12) | C25—C26—H26B | 109.5 |
N12—Co—N22i | 95.03 (8) | H26A—C26—H26B | 109.5 |
N12—Co—N22 | 95.03 (8) | C25—C26—H26C | 109.5 |
N22i—Co—N22 | 96.83 (8) | H26A—C26—H26C | 109.5 |
N12—Co—Cl | 121.33 (8) | H26B—C26—H26C | 109.5 |
N22i—Co—Cl | 121.09 (6) | C25—C26—H26D | 109.5 |
N22—Co—Cl | 121.09 (6) | H26A—C26—H26D | 141.1 |
N12—N11—B | 120.7 (2) | H26B—C26—H26D | 56.3 |
N22—N21—B | 120.93 (18) | H26C—C26—H26D | 56.3 |
N21i—B—N21 | 110.3 (2) | C25—C26—H26E | 109.5 |
N21i—B—N11 | 109.49 (17) | H26A—C26—H26E | 56.3 |
N21—B—N11 | 109.49 (17) | H26B—C26—H26E | 141.1 |
N11—N12—C13 | 107.0 (3) | H26C—C26—H26E | 56.3 |
N12—C13—C14 | 108.9 (3) | H26D—C26—H26E | 109.5 |
C13—C14—C15 | 106.9 (3) | C25—C26—H26F | 109.5 |
C14—C15—N11 | 107.7 (3) | H26A—C26—H26F | 56.3 |
C15—N11—N12 | 109.5 (2) | H26B—C26—H26F | 56.3 |
N21—N22—C23 | 106.77 (15) | H26C—C26—H26F | 141.1 |
N22—C23—C24 | 109.20 (19) | H26D—C26—H26F | 109.5 |
C23—C24—C25 | 106.85 (18) | H26E—C26—H26F | 109.5 |
C24—C25—N21 | 107.66 (18) | C23—C27—C28 | 109.5 (2) |
C25—N21—N22 | 109.52 (16) | C23—C27—C30 | 109.8 (2) |
N21—C25—C26 | 122.16 (18) | C28—C27—C30 | 109.1 (2) |
C14—C13—C17 | 129.5 (3) | C23—C27—C29 | 109.60 (18) |
N12—C13—C17 | 121.6 (3) | C28—C27—C29 | 108.3 (2) |
C15—C14—H14 | 126.6 | C30—C27—C29 | 110.5 (2) |
C13—C14—H14 | 126.6 | C27—C28—H28A | 109.5 |
N11—C15—C16 | 122.3 (3) | C27—C28—H28B | 109.5 |
C14—C15—C16 | 129.9 (3) | H28A—C28—H28B | 109.5 |
C15—C16—H16A | 108 (2) | C27—C28—H28C | 109.5 |
C15—C16—H16B | 108 (3) | H28A—C28—H28C | 109.5 |
H16A—C16—H16B | 113 (2) | H28B—C28—H28C | 109.5 |
C19—C17—C19i | 111.8 (3) | C27—C29—H29A | 109.5 |
C19—C17—C13 | 109.66 (18) | C27—C29—H29B | 109.5 |
C19i—C17—C13 | 109.66 (18) | H29A—C29—H29B | 109.5 |
C19—C17—C18 | 108.9 (2) | C27—C29—H29C | 109.5 |
C19i—C17—C18 | 108.9 (2) | H29A—C29—H29C | 109.5 |
C13—C17—C18 | 107.8 (3) | H29B—C29—H29C | 109.5 |
C17—C18—H18A | 109 (3) | C27—C30—H30A | 109.5 |
C17—C18—H18B | 109.7 (19) | C27—C30—H30B | 109.5 |
H18A—C18—H18B | 110 (2) | H30A—C30—H30B | 109.5 |
C17—C19—H19A | 109.5 | C27—C30—H30C | 109.5 |
C17—C19—H19B | 109.5 | H30A—C30—H30C | 109.5 |
H19A—C19—H19B | 109.5 | H30B—C30—H30C | 109.5 |
C17—C19—H19C | 109.5 | N21i—B—H1 | 108.8 (9) |
H19A—C19—H19C | 109.5 | N21—B—H1 | 108.8 (9) |
H19B—C19—H19C | 109.5 | N11—B—H1 | 109.9 (17) |
N22—C23—C27 | 122.62 (19) | C15—N11—B | 129.8 (3) |
C24—C23—C27 | 128.2 (2) | C13—N12—Co | 143.1 (2) |
C24—C25—C26 | 130.13 (19) | C25—N21—B | 129.55 (19) |
C25—C24—H24 | 126.6 | C23—N22—Co | 143.92 (17) |
C23—C24—H24 | 126.6 | ||
N12—C13—C14—C15 | 0 | C15—N11—N12—C13 | 0 |
C17—C13—C14—C15 | 180 | B—N11—N12—C13 | 180 |
C13—C14—C15—N11 | 0 | C15—N11—N12—Co | 180 |
C13—C14—C15—C16 | 180 | B—N11—N12—Co | 0 |
N12—C13—C17—C19 | −61.6 (2) | C24—C25—N21—N22 | −0.6 (2) |
C14—C13—C17—C19 | 118.4 (2) | C26—C25—N21—N22 | 177.14 (19) |
N12—C13—C17—C19i | 61.6 (2) | C24—C25—N21—B | 179.8 (2) |
C14—C13—C17—C19i | −118.4 (2) | C26—C25—N21—B | −2.4 (3) |
N12—C13—C17—C18 | 180 | N21i—B—N21—C25 | 118.2 (2) |
C14—C13—C17—C18 | 0 | N11—B—N21—C25 | −121.3 (2) |
N22—C23—C24—C25 | −0.4 (3) | N21i—B—N21—N22 | −61.4 (3) |
C27—C23—C24—C25 | −179.5 (2) | N11—B—N21—N22 | 59.2 (3) |
C23—C24—C25—N21 | 0.6 (3) | C24—C23—N22—N21 | 0.1 (3) |
C23—C24—C25—C26 | −176.9 (2) | C27—C23—N22—N21 | 179.17 (19) |
N22—C23—C27—C28 | 179.7 (2) | C24—C23—N22—Co | 177.5 (2) |
C24—C23—C27—C28 | −1.4 (4) | C27—C23—N22—Co | −3.4 (4) |
N22—C23—C27—C30 | −60.5 (3) | C25—N21—N22—C23 | 0.3 (2) |
C24—C23—C27—C30 | 118.4 (3) | B—N21—N22—C23 | 180.0 (2) |
N22—C23—C27—C29 | 61.1 (3) | C25—N21—N22—Co | −178.08 (14) |
C24—C23—C27—C29 | −120.0 (3) | B—N21—N22—Co | 1.5 (2) |
C14—C15—N11—N12 | 0 | C13—N12—Co—N22i | 131.34 (4) |
C16—C15—N11—N12 | 180 | N11—N12—Co—N22i | −48.66 (4) |
C14—C15—N11—B | 180 | C13—N12—Co—N22 | −131.34 (4) |
C16—C15—N11—B | 0 | N11—N12—Co—N22 | 48.66 (4) |
N21i—B—N11—C15 | −119.48 (16) | C13—N12—Co—Cl | 0 |
N21—B—N11—C15 | 119.48 (17) | N11—N12—Co—Cl | 180 |
N21i—B—N11—N12 | 60.52 (16) | C23—N22—Co—N12 | 133.0 (3) |
N21—B—N11—N12 | −60.52 (16) | N21—N22—Co—N12 | −49.55 (14) |
C14—C13—N12—N11 | 0 | C23—N22—Co—N22i | −131.3 (2) |
C17—C13—N12—N11 | 180 | N21—N22—Co—N22i | 46.1 (2) |
C14—C13—N12—Co | 180 | C23—N22—Co—Cl | 1.5 (3) |
C17—C13—N12—Co | 0 | N21—N22—Co—Cl | 178.95 (11) |
Symmetry code: (i) −x+1/2, y, z. |
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