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_4346381
_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 Cu2 N7 O2, 1.39(C H2 Cl2), C F3 O3 S, C1 H4 O1'
_chemical_formula_sum            'C67.39 H76.79 Cl2.79 Cu2 F3 N7 O6 S'
_chemical_formula_weight         1395.85
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-29
_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                 99.1436(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.69383(18)
_cell_length_b                   24.2156(3)
_cell_length_c                   21.4722(2)
_cell_measurement_reflns_used    28651
_cell_measurement_temperature    99.8(4)
_cell_measurement_theta_max      73.5180
_cell_measurement_theta_min      3.9970
_cell_volume                     7029.80(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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.8(4)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega  -71.00   31.00   1.0000    1.3000
omega____ theta____ kappa____ phi______ frames
    -      -40.9351   57.0000 -120.0000 102

  2 omega -110.00  -25.00   1.0000    1.3000
omega____ theta____ kappa____ phi______ frames
    -      -40.9351  -57.0000   90.0000 85

  3 omega -140.00 -107.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -94.0000  -90.0000 33

  4 omega   31.00   90.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -30.0000 -150.0000 59

  5 omega  140.00  166.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      107.0326    0.0000 -180.0000 26

  6 omega   38.00   96.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -45.0000    0.0000 58

  7 omega  146.00  173.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  125.0000 -150.0000 27

  8 omega   29.00   82.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -30.0000  -60.0000 53

  9 omega   29.00   55.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -30.0000  120.0000 26

 10 omega   19.00  137.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      107.0326    0.0000 -180.0000 118

 11 omega  111.00  152.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  125.0000   90.0000 41

 12 omega   35.00   98.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -45.0000   60.0000 63

 13 omega -115.00  -11.00   1.0000    1.3000
omega____ theta____ kappa____ phi______ frames
    -      -40.9351  -57.0000 -120.0000 104

 14 omega -115.00  -11.00   1.0000    1.3000
omega____ theta____ kappa____ phi______ frames
    -      -40.9351  -57.0000  -30.0000 104

 15 omega -134.00  -22.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -77.0000 -180.0000 112

 16 omega   32.00  121.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      107.0326 -125.0000  -90.0000 89

 17 omega   77.00  178.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   30.0000 -120.0000 101

 18 omega   73.00  178.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   77.0000   30.0000 105

 19 omega   23.00  109.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -94.0000    0.0000 86

 20 omega   46.00  178.00   1.0000    5.2000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   15.0000    0.0000 132

 21 omega   23.00   98.00   1.0000    1.3000
omega____ theta____ kappa____ phi______ frames
    -       40.9351 -125.0000   90.0000 75
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0124457000
_diffrn_orient_matrix_UB_12      0.0056895000
_diffrn_orient_matrix_UB_13      -0.0723029000
_diffrn_orient_matrix_UB_21      -0.0652031000
_diffrn_orient_matrix_UB_22      -0.0521722000
_diffrn_orient_matrix_UB_23      -0.0074469000
_diffrn_orient_matrix_UB_31      -0.0926402000
_diffrn_orient_matrix_UB_32      0.0358876000
_diffrn_orient_matrix_UB_33      0.0008483000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66840
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.82
_diffrn_reflns_theta_min         3.27
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.500
_exptl_absorpt_correction_T_max  0.715
_exptl_absorpt_correction_T_min  0.400
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2906
_exptl_crystal_size_max          0.4365
_exptl_crystal_size_mid          0.2309
_exptl_crystal_size_min          0.1156
_refine_diff_density_max         1.459
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         14010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1040P)^2^+7.2485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1640
_refine_ls_wR_factor_ref         0.1716
_reflns_number_gt                12351
_reflns_number_total             14010
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01380_si_002.cif
_cod_data_source_block           complex2
_cod_original_cell_volume        7029.79(15)
_cod_database_code               4346381
_chemical_oxdiff_formula         'Cu2 C64 N7 H70 C4 H8 Cl8'
_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, All O(H) groups
2. Others
 Sof(Cl1)=Sof(Cl2)=Sof(C1S)=Sof(H1SB)=Sof(H1SC)=FVAR(1)
 Sof(Cl3)=Sof(Cl4)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=FVAR(2)
 Sof(O1SA)=Sof(H1SA)=Sof(C3SA)=Sof(H3SA)=Sof(H3SB)=Sof(H3SC)=1-FVAR(3)
 Sof(O1S)=Sof(H1S)=Sof(C3S)=Sof(H3SD)=Sof(H3SE)=Sof(H3SF)=FVAR(3)
3.a Secondary CH2 refined with riding coordinates:
 C1S(H1SB,H1SC), C2S(H2SA,H2SB)
3.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), 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)
3.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), C3SA(H3SA,H3SB,
 H3SC), C3S(H3SD,H3SE,H3SF)
3.d Idealised tetrahedral OH refined as rotating group:
 O1SA(H1SA), O1S(H1S)
;
_olex2_submission_special_instructions 'No special instructions were received'