Methylene-bridged bimetallic bis(imino)pyridine-cobaltous chlorides as precatalysts for vinyl-terminated polyethylene waxes.
Chen, Qiang; Zhang, Wenjuan; Solan, Gregory A.; Liang, Tongling; Sun, Wen-Hua; Dalton transactions (Cambridge, England : 2003) 47 (2018) 6124–6133; doi:10.1039/c8dt00907d

data_7045996
_publ_section_title
;
 Methylene-bridged bimetallic bis(imino)pyridine-cobaltous chlorides as
 precatalysts for vinyl-terminated polyethylene waxes.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6124
_journal_page_last               6133
_journal_paper_doi               10.1039/c8dt00907d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C57 H58 Cl4 Co2 N6 O'
_chemical_formula_sum            'C57 H58 Cl4 Co2 N6 O'
_chemical_formula_weight         1102.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-07 deposited with the CCDC.
2018-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.102(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.2036(5)
_cell_length_b                   24.5959(6)
_cell_length_c                   34.1168(11)
_cell_measurement_reflns_used    19243
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.3290
_cell_measurement_theta_min      1.6060
_cell_volume                     12725.2(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1344
_diffrn_reflns_av_unetI/netI     0.1722
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            85709
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.628
_diffrn_reflns_theta_min         1.578
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74185
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       block
_exptl_crystal_F_000             4576.0
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.032
_platon_squeeze_details
;
TITL mx6465d_a.res in C2/c
CELL   15.2036   24.5959   34.1168     90.00     94.10     90.00
SPGR C2/c
Q101 0.966 0.041 0.349 !       3.71 eA-3
C102 0.038 0.157 0.845 !       3.29 eA-3
C103 0.486 0.077 0.257 !       2.20 eA-3
C104 0.500 0.047 0.252 !       1.99 eA-3
C105 0.468 0.332 0.136 !       1.92 eA-3
C106 0.495 0.497 0.376 !       1.83 eA-3
C107 0.458 0.040 0.219 !       1.81 eA-3
C108 0.497 0.044 0.229 !       1.75 eA-3
C109 0.449 0.345 0.110 !       1.72 eA-3
C110 0.559 0.313 0.340 !       1.70 eA-3
C111 0.964 0.190 0.680 !       1.60 eA-3
C112 0.609 0.317 0.353 !       1.58 eA-3
C113 0.108 0.176 0.850 !       1.58 eA-3
C114 0.501 0.353 0.361 !       1.57 eA-3
C115 0.562 0.063 0.290 !       1.56 eA-3
C116 0.455 0.077 0.242 !       1.56 eA-3
C117 0.500 0.021 0.234 !       1.54 eA-3
C118 0.954 0.405 0.696 !       1.48 eA-3
C119 0.504 0.321 0.344 !       1.46 eA-3
C120 0.488 0.069 0.180 !       1.43 eA-3
C121 0.518 0.063 0.288 !       1.43 eA-3
C122 0.072 0.443 0.813 !       1.39 eA-3
C123 0.433 0.095 0.218 !       1.39 eA-3
C124 0.406 0.342 0.162 !       1.37 eA-3
C125 0.482 0.258 0.235 !       1.36 eA-3
C126 0.577 0.254 0.272 !       1.35 eA-3
C127 0.420 0.089 0.172 !       1.34 eA-3
C128 0.080 0.411 0.828 !       1.34 eA-3
Q129 0.092 0.077 0.170 !       1.30 eA-3
C130 0.398 0.111 0.195 !       1.29 eA-3
C131 0.522 0.333 0.321 !       1.29 eA-3
C132 0.602 0.234 0.296 !       1.27 eA-3
C133 0.435 0.285 0.166 !       1.25 eA-3
C134 0.603 0.081 0.305 !       1.24 eA-3
C135 0.050 0.500 0.274 !       1.23 eA-3
Q136 0.495 0.463 0.828 !       1.20 eA-3
C137 0.418 0.258 0.196 !       1.20 eA-3
C138 0.317 0.128 0.173 !       1.20 eA-3
C139 0.543 0.271 0.323 !       1.18 eA-3
Q140 0.297 0.280 0.970 !       1.18 eA-3
C141 0.952 0.479 0.763 !       1.18 eA-3
C142 0.457 0.023 0.242 !       1.17 eA-3
Q143 0.797 0.036 0.325 !       1.17 eA-3
C144 0.010 0.127 0.843 !       1.17 eA-3
C145 0.506 0.388 0.372 !       1.15 eA-3
C146 0.882 0.300 0.702 !       1.15 eA-3
C147 0.423 0.146 0.194 !       1.13 eA-3
C148 0.377 0.309 0.174 !       1.12 eA-3
C149 0.407 0.176 0.205 !       1.12 eA-3
C150 0.449 0.275 0.209 !       1.11 eA-3
C151 0.955 0.435 0.784 !       1.10 eA-3
C152 0.434 0.340 0.329 !       1.10 eA-3
C153 0.511 0.330 0.273 !       1.09 eA-3
Q154 0.996 0.770 0.331 !       1.09 eA-3
Q155 0.496 0.270 0.331 !       1.09 eA-3
C156 0.420 0.076 0.266 !       1.08 eA-3
Q157 0.251 0.124 0.398 !       1.08 eA-3
C158 0.456 0.402 0.133 !       1.07 eA-3
C159 1.005 0.030 0.600 !       1.06 eA-3
C160 0.157 0.259 0.782 !       1.05 eA-3
C161 0.508 0.329 0.295 !       1.05 eA-3
Q162 0.396 0.358 0.126 !       1.05 eA-3
C163 0.432 0.375 0.153 !       1.04 eA-3
C164 0.530 0.302 0.281 !       1.04 eA-3
C165 0.506 0.291 0.297 !       1.04 eA-3
C166 0.520 0.501 0.406 !       1.03 eA-3
Q167 0.629 0.144 0.655 !       1.03 eA-3
Q168 0.233 0.070 0.188 !       1.03 eA-3
Q169 0.565 0.384 0.062 !       1.03 eA-3
C170 0.525 0.228 0.267 !       1.02 eA-3
Q171 0.566 0.025 0.139 !       1.02 eA-3
C172 0.971 0.494 0.251 !       1.02 eA-3
Q173 0.262 0.461 0.022 !       1.02 eA-3
C174 0.654 0.094 0.329 !       1.01 eA-3
C175 0.987 0.482 0.798 !       1.01 eA-3
Q176 0.037 0.005 0.584 !       1.00 eA-3
Q177 0.886 0.376 0.758 !       1.00 eA-3
C178 0.559 0.051 0.149 !       1.00 eA-3
Q179 0.107 0.440 0.672 !       1.00 eA-3
C180 0.621 0.064 0.328 !       1.00 eA-3
Q181 0.673 0.232 0.219 !       1.00 eA-3
Q182 0.044 0.438 0.344 !       1.00 eA-3
Q183 0.047 0.468 0.883 !       0.99 eA-3
Q184 0.688 0.149 0.540 !       0.99 eA-3
C185 0.527 0.032 0.308 !       0.99 eA-3
C186 0.580 0.223 0.274 !       0.99 eA-3
Q187 1.003 0.156 0.915 !       0.99 eA-3
C188 0.473 0.315 0.311 !       0.97 eA-3
Q189 0.254 0.056 0.267 !       0.97 eA-3
C190 0.530 0.252 0.282 !       0.97 eA-3
C191 0.486 0.349 0.382 !       0.97 eA-3
C192 0.139 0.271 0.822 !       0.97 eA-3
Q193 0.406 0.144 0.141 !       0.97 eA-3
Q194 0.842 0.222 0.041 !       0.97 eA-3
Q195 0.643 0.290 0.025 !       0.97 eA-3
Q196 0.404 0.120 0.350 !       0.97 eA-3
C197 0.113 0.102 0.163 !       0.97 eA-3
Q198 0.202 0.194 0.157 !       0.96 eA-3
C199 0.397 0.191 0.222 !       0.96 eA-3
;
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         19779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.2230
_refine_ls_R_factor_gt           0.0938
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1076P)^2^+0.4071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2161
_refine_ls_wR_factor_ref         0.2755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7837
_reflns_number_total             19779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00907d2.cif
_cod_data_source_block           Co
_cod_depositor_comments          'Adding full bibliography for 7045996.cif.'
_cod_database_code               7045996
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.916
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C18(H18)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C36(H36), C12(H12), C38(H38), C37(H37), C14(H14), C26(H26), C52(H52),
 C20(H20), C44(H44), C30(H30), C54(H54), C21(H21), C46(H46), C5(H5), C45(H45),
 C53(H53), C24(H24), C6(H6), C23(H23)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C56(H56a,H56b,H56c), C48(H48a,H48b,H48c), C41(H41a,H41b,
 H41c), C34(H34a,H34b,H34c), C17(H17a,H17b,H17c), C49(H49a,H49b,H49c), C31(H31a,
 H31b,H31c), C32(H32a,H32b,H32c), C16(H16a,H16b,H16c), C57(H57a,H57b,H57c),
 C9(H9a,H9b,H9c)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'