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_4346383
_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 H70 Co2 N7 O2, 1.04(Cl O4), 1.58(C3 H6 O), 0.56(C H4 O), C H3 O'
_chemical_formula_sum            'C70.3 H84.72 Cl1.04 Co2 N7 O9.3'
_chemical_formula_weight         1331.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.4205(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.58121(17)
_cell_length_b                   24.3465(3)
_cell_length_c                   21.1737(2)
_cell_measurement_reflns_used    26686
_cell_measurement_temperature    99.95(10)
_cell_measurement_theta_max      73.5220
_cell_measurement_theta_min      3.9970
_cell_volume                     6885.72(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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., 2013)'
_diffrn_ambient_temperature      99.95(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega -120.00   -8.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9351  -77.0000 -180.0000 112

  2 omega  -46.00   35.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9351   37.0000  -60.0000 81

  3 omega -115.00  -82.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -94.0000  150.0000 33

  4 omega -128.00  -88.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000 -125.0000    0.0000 40

  5 omega   77.00  174.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   77.0000 -150.0000 97

  6 omega   37.00   64.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -30.0000   90.0000 27

  7 omega   31.00   72.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -30.0000 -120.0000 41

  8 omega  147.00  174.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  125.0000  -60.0000 27

  9 omega  114.00  177.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   30.0000  120.0000 63

 10 omega  103.00  129.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  125.0000  -60.0000 26

 11 omega   53.00  103.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -94.0000   90.0000 50

 12 omega   45.00   97.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -45.0000  120.0000 52

 13 omega   88.00  157.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   45.0000    0.0000 69

 14 omega -115.00  -11.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9351  -57.0000  -60.0000 104

 15 omega -120.00   -7.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9351  -77.0000   60.0000 113

 16 omega    1.00   83.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9351  -99.0000   30.0000 82

 17 omega -130.00  -85.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -61.0000 -120.0000 45

 18 omega   77.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   30.0000   60.0000 101

 19 omega   73.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   77.0000  -90.0000 105

 20 omega   29.00   90.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -30.0000  -60.0000 61

 21 omega   77.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   61.0000  -30.0000 101

 22 omega   73.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   77.0000  150.0000 105

 23 omega   23.00  109.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -94.0000  -90.0000 86
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0474398000
_diffrn_orient_matrix_UB_12      -0.0533694000
_diffrn_orient_matrix_UB_13      0.0307101000
_diffrn_orient_matrix_UB_21      -0.0274854000
_diffrn_orient_matrix_UB_22      0.0169383000
_diffrn_orient_matrix_UB_23      0.0647442000
_diffrn_orient_matrix_UB_31      -0.1014482000
_diffrn_orient_matrix_UB_32      -0.0294979000
_diffrn_orient_matrix_UB_33      -0.0183615000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66905
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.66
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.630
_exptl_absorpt_correction_T_max  0.608
_exptl_absorpt_correction_T_min  0.428
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2806
_exptl_crystal_size_max          0.3313
_exptl_crystal_size_mid          0.2351
_exptl_crystal_size_min          0.1703
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         13740
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0642P)^2^+7.1659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1317
_reflns_number_gt                12826
_reflns_number_total             13740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01380_si_002.cif
_cod_data_source_block           complex4
_cod_original_cell_volume        6885.74(15)
_cod_original_formula_sum        'C70.30 H84.72 Cl1.04 Co2 N7 O9.30'
_cod_database_code               4346383
_chemical_oxdiff_formula         'C64 H70 Cl Co2 N7 O6 C2 H8 O2 C6 H12 O2'
_reflns_odcompleteness_completeness 99.96
_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, All O(H) groups
2. Rigid bond restraints
 C5S, C4S, C6S, O2S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2, O7, O10, O8, O9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Same fragment restrains
{O1S, C1S, C2S, C3S}
as
{O2S, C4S, C5S, C6S}
{O1S, C1S, C2S, C3S}
as
{O2SA, C4SA, C5SA, C6SA}
4. Others
 Sof(O1S)=Sof(C1S)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(H2SC)=Sof(C3S)=Sof(H3SA)=
 Sof(H3SB)=Sof(H3SC)=FVAR(1)
 Sof(O2S)=Sof(C4S)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(H5SC)=Sof(C6S)=Sof(H6SA)=
 Sof(H6SB)=Sof(H6SC)=1-FVAR(2)
 Sof(Cl2)=Sof(O7)=Sof(O8)=Sof(O9)=Sof(O10)=FVAR(2)
 Sof(O3S)=Sof(H3S)=Sof(C7S)=Sof(H7SA)=Sof(H7SB)=Sof(H7SC)=FVAR(3)
 Sof(O2SA)=Sof(C4SA)=Sof(C5SA)=Sof(H5SD)=Sof(H5SE)=Sof(H5SF)=Sof(C6SA)=
 Sof(H6SD)=Sof(H6SE)=Sof(H6SF)=1-FVAR(4)
 Sof(Cl1)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=FVAR(4)
 Fixed Sof: O4S(0.5) C8S(0.5) H8SA(0.5) H8SB(0.5) H8SC(0.5) O4SA(0.5)
 C8SA(0.5) H8SD(0.5) H8SE(0.5) H8SF(0.5)
5.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), C47(H47), C48(H48),
  C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57),
 C58(H58), C61(H61), C62(H62), C63(H63), C64(H64)
5.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), C2S(H2SA,H2SB,
 H2SC), C3S(H3SA,H3SB,H3SC), C5S(H5SA,H5SB,H5SC), C6S(H6SA,H6SB,H6SC), C7S(H7SA,
 H7SB,H7SC), C8S(H8SA,H8SB,H8SC), C8SA(H8SD,H8SE,H8SF), C5SA(H5SD,H5SE,H5SF),
 C6SA(H6SD,H6SE,H6SF)
5.c Idealised tetrahedral OH refined with riding coordinates:
 O3S(H3S)
;
_olex2_submission_special_instructions 'No special instructions were received'