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_4346384
_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 O2, Cl O4, 2(C H4 O)'
_chemical_formula_sum            'C66 H74 Br4 Cl Co2 N7 O8'
_chemical_formula_weight         1566.27
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                103.5940(19)
_cell_angle_beta                 90.9765(18)
_cell_angle_gamma                93.6981(19)
_cell_formula_units_Z            2
_cell_length_a                   11.7740(3)
_cell_length_b                   13.3797(3)
_cell_length_c                   21.9485(5)
_cell_measurement_reflns_used    20417
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.0540
_cell_measurement_theta_min      3.3700
_cell_volume                     3351.89(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    'XS (Sheldrick, 2008)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.979
_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    -71.00  32.00   1.00    1.00    --  -41.52  57.00-120.00  103
  2  \w   -124.00 -79.00   1.00    1.00    --  -41.52 -99.00-150.00   45
  3  \w   -124.00 -79.00   1.00    1.00    --  -41.52 -99.00 150.00   45
  4  \w   -115.00 -12.00   1.00    1.00    --  -41.52 -57.00  90.00  103
  5  \w      1.00  83.00   1.00    1.00    --   41.52 -99.00  30.00   82
  6  \w     23.00  99.00   1.00    1.00    --   41.52-125.00 -30.00   76
  7  \w     34.00 139.00   1.00    3.04    --  108.29 -61.00 120.00  105
  8  \w     33.00 122.00   1.00    3.04    --  108.29-125.00 -60.00   89
  9  \w     78.00 178.00   1.00    3.04    --  108.29  30.00   0.00  100
 10  \w     75.00 178.00   1.00    3.04    --  108.29  77.00 120.00  103
 11  \w     78.00 178.00   1.00    3.04    --  108.29  30.00  90.00  100
 12  \w     94.00 178.00   1.00    3.04    --  108.29 125.00 -30.00   84
 13  \w     34.00 136.00   1.00    3.04    --  108.29 -45.00 -30.00  102
 14  \w     78.00 178.00   1.00    3.04    --  108.29  30.00-150.00  100
 15  \w     24.00 109.00   1.00    3.04    --  108.29 -94.00 -30.00   85
 16  \w     24.00 109.00   1.00    3.04    --  108.29 -94.00  30.00   85
 17  \w     24.00 109.00   1.00    3.04    --  108.29 -94.00 120.00   85
 18  \w     94.00 178.00   1.00    3.04    --  108.29 125.00   0.00   84
 19  \w     24.00 109.00   1.00    3.04    --  108.29 -94.00 -60.00   85
 20  \w   -124.00 -79.00   1.00    1.00    --  -41.52 -99.00 -60.00   45
 21  \w   -124.00 -79.00   1.00    1.00    --  -41.52 -99.00   0.00   45
 22  \w   -115.00 -12.00   1.00    1.00    --  -41.52 -57.00 -90.00  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      0.0196035000
_diffrn_orient_matrix_UB_12      -0.0978008000
_diffrn_orient_matrix_UB_13      0.0232082000
_diffrn_orient_matrix_UB_21      0.1230792000
_diffrn_orient_matrix_UB_22      0.0420227000
_diffrn_orient_matrix_UB_23      0.0205787000
_diffrn_orient_matrix_UB_31      -0.0409630000
_diffrn_orient_matrix_UB_32      0.0526496000
_diffrn_orient_matrix_UB_33      0.0652561000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37783
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.14
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.510
_exptl_absorpt_correction_T_max  0.693
_exptl_absorpt_correction_T_min  0.311
_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    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.299
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         13369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+2.4132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                12546
_reflns_number_total             13369
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01380_si_002.cif
_cod_data_source_block           complex5
_cod_original_cell_volume        3351.89(13)
_cod_database_code               4346384
_chemical_oxdiff_formula         'Co2 C54 H58 N7 O6 Cl Br2 (C H4 O)2'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O3A)
Uiso(O6A) = Uiso(O5A) = Uiso(O4A)
3. Others
 Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=1-FVAR(1)
 Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=FVAR(1)
4.a 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)
4.b 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), C65(H65A,H65B,
 H65C), C66(H66A,H66B,H66C)
;
_olex2_date_sample_data_collection 2015-05-26
_olex2_date_sample_submission    2015-05-26
_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 1.506
_oxdiff_exptl_absorpt_empirical_full_min 0.725