Crystal structure of bis(μ3-chlorido)-bis(μ2-chlorido)-tetrakis(μ2-2,6-bis (diphenylmethyl)-4-t-butylphenolato)tetralithium(I)dicobalt(II) toluene solvate, C75.5H70Cl2CoLi2O2
Bu, Donglei; Chen, Xiaodan; Meng, Miao; Zhu, Feifeng; Lei, Hao; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 239–241; doi:10.1515/ncrs-2017-0238

data_8106111
_publ_section_title
;
 Crystal structure of
 bis(\m3-chlorido)-bis(\m2-chlorido)-tetrakis(\m2-2,6-bis
 (diphenylmethyl)-4-t-butylphenolato)tetralithium(I)dicobalt(II) toluene
 solvate, C75.5H70Cl2CoLi2O2
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              239
_journal_page_last               241
_journal_paper_doi               10.1515/ncrs-2017-0238
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C144 H132 Cl4 Co2 Li4 O4, C7 H8'
_chemical_formula_sum            'C151 H140 Cl4 Co2 Li4 O4'
_chemical_formula_weight         2306.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                88.604(5)
_cell_angle_beta                 88.255(4)
_cell_angle_gamma                68.282(5)
_cell_formula_units_Z            1
_cell_length_a                   13.1085(7)
_cell_length_b                   13.4704(7)
_cell_length_c                   18.8367(10)
_cell_measurement_reflns_used    4931
_cell_measurement_temperature    150
_cell_measurement_theta_max      62.8220
_cell_measurement_theta_min      4.0010
_cell_volume                     3088.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0288
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
  1 omega -109.00  -83.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -      -33.1184 -178.0000    0.0000 26

  2 omega    2.00   94.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       33.1184 -133.0000  -23.0000 92

  3 omega   35.00   85.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       33.1184  178.0000   90.0000 50

  4 omega  -35.00  -10.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       33.1184  -77.0000 -180.0000 25

  5 omega   14.00  101.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       33.1184   57.0000 -150.0000 87

  6 omega    8.00  106.00   1.0000    1.2500
omega____ theta____ kappa____ phi______ frames
    -       33.1184   38.0000  120.0000 98

  7 omega   29.00  139.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000    0.0000  -90.0000 110

  8 omega   25.00   60.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000    0.0000 35

  9 omega   49.00  126.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000 -105.8032 77

 10 omega   23.00   58.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000   60.0000 35

 11 omega   82.00  107.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000  -61.7350 25

 12 omega   22.00   73.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000 -180.0000 51

 13 omega   38.00   74.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000  -60.0000 36

 14 omega   19.00   65.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000  120.0000 46

 15 omega   67.00  153.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   45.0000  -60.0000 86

 16 omega   43.00   68.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000  -61.7350 25

 17 omega   39.00  118.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000  133.0313 79

 18 omega   22.00   61.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -94.0000 -150.0000 39

 19 omega   25.00   70.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000  -90.0000 45

 20 omega   49.00  124.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  178.0000 -180.0000 75

 21 omega   20.00   70.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -92.0000   38.9093 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0201957000
_diffrn_orient_matrix_UB_12      0.0108121000
_diffrn_orient_matrix_UB_13      -0.0804570000
_diffrn_orient_matrix_UB_21      0.1239898000
_diffrn_orient_matrix_UB_22      -0.0579079000
_diffrn_orient_matrix_UB_23      -0.0148815000
_diffrn_orient_matrix_UB_31      -0.0151767000
_diffrn_orient_matrix_UB_32      -0.1081092000
_diffrn_orient_matrix_UB_33      0.0012380000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.1089
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16983
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        62.642
_diffrn_reflns_theta_max         62.641
_diffrn_reflns_theta_min         3.532
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.324
_exptl_absorpt_correction_T_max  0.717
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       block
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         9602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+0.9840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1743
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5988
_reflns_number_total             9602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0238_suppl.cif
_cod_data_source_block           lh_141203_2
_cod_database_code               8106111
_reflns_odcompleteness_completeness 98.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C80(0.5) H80A(0.5) H80B(0.5) H80C(0.5) C74(0.5) C75(0.5) H75(0.5)
 C76(0.5) H76(0.5) C77(0.5) H77(0.5) C78(0.5) H78(0.5) C79(0.5) H79(0.5)
3.a Ternary CH refined with riding coordinates:
 C43(H43), C61(H61), C7(H7), C24(H24)
3.b Aromatic/amide H refined with riding coordinates:
 C73(H73), C36(H36), C39(H39), C3(H3), C67(H67), C5(H5), C56(H56), C71(H71),
 C26(H26), C50(H50), C41(H41), C33(H33), C46(H46), C19(H19), C72(H72), C15(H15),
  C9(H9), C55(H55), C69(H69), C34(H34), C52(H52), C63(H63), C32(H32), C18(H18),
 C54(H54), C13(H13), C47(H47), C65(H65), C64(H64), C30(H30), C35(H35), C12(H12),
  C70(H70), C53(H53), C66(H66), C48(H48), C16(H16), C49(H49), C29(H29),
 C10(H10), C11(H11), C17(H17), C27(H27), C28(H28), C75(H75), C76(H76), C77(H77),
  C78(H78), C79(H79)
3.c Fitted hexagon refined as free rotating group:
 C74(C75,C76,C77,C78,C79)
3.d Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C23(H23A,H23B,
 H23C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C80(H80A,H80B,H80C)
;
_shelx_res_checksum              14226
_shelx_hkl_checksum              94529
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'