Bimetallic Complexes Supported by a Redox-Active Ligand with Fused Pincer-Type Coordination Sites.
Wang, Denan; Lindeman, Sergey V.; Fiedler, Adam T.; Inorganic chemistry 54 (2015) 8744–8754; doi:10.1021/acs.inorgchem.5b01380

data_4346385
_publ_section_title
;
 Bimetallic Complexes Supported by a Redox-Active Ligand with Fused
 Pincer-Type Coordination Sites.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8744
_journal_page_last               8754
_journal_paper_doi               10.1021/acs.inorgchem.5b01380
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C64 H66 Br4 Co2 N7 O4, Cl O4, 2(C H2 Cl2)'
_chemical_formula_sum            'C66 H70 Br4 Cl5 Co2 N7 O8'
_chemical_formula_weight         1704.04
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                81.9458(15)
_cell_angle_beta                 89.9831(16)
_cell_angle_gamma                71.562(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1787(3)
_cell_length_b                   13.8609(3)
_cell_length_c                   22.2351(3)
_cell_measurement_reflns_used    22491
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.0730
_cell_measurement_theta_min      3.9560
_cell_volume                     3810.96(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -68.00  35.00   1.00    4.00    --  -41.40  37.00  90.00  103
  2  \w    -96.00  -2.00   1.00    4.00    --  -41.40 125.00-120.00   94
  3  \w    -68.00  35.00   1.00    4.00    --  -41.40  37.00-180.00  103
  4  \w   -124.00 -79.00   1.00    4.00    --  -41.40 -99.00  60.00   45
  5  \w   -124.00 -79.00   1.00    4.00    --  -41.40 -99.00 120.00   45
  6  \w     23.00  99.00   1.00    4.00    --   41.40-125.00 -90.00   76
  7  \w     23.00  99.00   1.00    4.00    --   41.40-125.00  60.00   76
  8  \w     94.00 178.00   1.00   16.00    --  108.29 125.00 -60.00   84
  9  \w     78.00 178.00   1.00   16.00    --  108.29  30.00  90.00  100
 10  \w     78.00 178.00   1.00   16.00    --  108.29  61.00 -90.00  100
 11  \w     94.00 178.00   1.00   16.00    --  108.29 125.00 -90.00   84
 12  \w     24.00 109.00   1.00   16.00    --  108.29 -94.00 -30.00   85
 13  \w     34.00 139.00   1.00   16.00    --  108.29 -61.00   0.00  105
 14  \w     33.00 122.00   1.00   16.00    --  108.29-125.00-120.00   89
 15  \w     30.00 139.00   1.00   16.00    --  108.29 -30.00-180.00  109
 16  \w     34.00 136.00   1.00   16.00    --  108.29 -45.00 -60.00  102
 17  \w     30.00 142.00   1.00   16.00    --  108.29 -77.00-150.00  112
 18  \w     33.00 122.00   1.00   16.00    --  108.29-125.00 120.00   89
 19  \w     81.00 178.00   1.00   16.00    --  108.29  45.00   0.00   97
 20  \w   -120.00  -8.00   1.00    4.00    --  -41.40 -77.00   0.00  112
 21  \w   -120.00  -8.00   1.00    4.00    --  -41.40 -77.00-150.00  112
 22  \w   -115.00 -12.00   1.00    4.00    --  -41.40 -57.00 120.00  103
 23  \w   -115.00 -12.00   1.00    4.00    --  -41.40 -57.00-120.00  103
 24  \w   -115.00 -12.00   1.00    4.00    --  -41.40 -57.00   0.00  103
 25  \w     75.00 178.00   1.00   16.00    --  108.29  77.00-150.00  103
 26  \w     75.00 178.00   1.00   16.00    --  108.29  77.00  60.00  103
 27  \w     78.00 178.00   1.00   16.00    --  108.29  30.00-180.00  100
 28  \w     78.00 178.00   1.00   16.00    --  108.29  61.00-180.00  100
 29  \w     78.00 178.00   1.00   16.00    --  108.29  61.00  30.00  100
 30  \w     81.00 178.00   1.00   16.00    --  108.29  45.00 120.00   97
 31  \w     78.00 178.00   1.00   16.00    --  108.29  61.00-120.00  100
 32  \w     78.00 178.00   1.00   16.00    --  108.29  61.00   0.00  100
 33  \w     75.00 178.00   1.00   16.00    --  108.29  77.00 -60.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1072410000
_diffrn_orient_matrix_UB_12      0.0126851000
_diffrn_orient_matrix_UB_13      -0.0206501000
_diffrn_orient_matrix_UB_21      -0.0209824000
_diffrn_orient_matrix_UB_22      -0.0260655000
_diffrn_orient_matrix_UB_23      -0.0629818000
_diffrn_orient_matrix_UB_31      -0.0572420000
_diffrn_orient_matrix_UB_32      0.1148548000
_diffrn_orient_matrix_UB_33      -0.0226761000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            71885
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.22
_diffrn_reflns_theta_min         3.54
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.915
_exptl_absorpt_correction_T_max  0.737
_exptl_absorpt_correction_T_min  0.332
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.30a (Agilent, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.049
_refine_diff_density_max         1.838
_refine_diff_density_min         -1.546
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     843
_refine_ls_number_reflns         15266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0730
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1245P)^2^+5.6095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2090
_refine_ls_wR_factor_ref         0.2197
_reflns_number_gt                12514
_reflns_number_total             15266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01380_si_002.cif
_cod_data_source_block           complex5-O2
_cod_original_cell_volume        3810.93(13)
_cod_database_code               4346385
_chemical_oxdiff_formula         'Co2 C65 H72 N7 O6 Br2 Cl (C H2 Cl2)2 O2'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C18(H18), C19(H19), C21(H21), C26(H26), C28(H28),
 C29(H29), C40(H40), C41(H41), C43(H43), C45(H45), C46(H46), C48(H48), C51(H51),
  C53(H53), C54(H54), C55(H55), C56(H56), C58(H58), C61(H61), C63(H63), C64(H64)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C44(H44A,H44B,H44C)
;
_olex2_date_sample_data_collection 2015-05-20
_olex2_date_sample_submission    2015-05-19
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.378
_oxdiff_exptl_absorpt_empirical_full_min 0.715