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_4346380
_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
'C61 H74 Cu2 N7 O3, C F3 O3 S, 1.43(C1 H4 O1), 0.07(C H2 Cl2)'
_chemical_formula_sum            'C63.5 H79.86 Cl0.14 Cu2 F3 N7 O7.43 S'
_chemical_formula_weight         1281.15
_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             2014-10-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                83.0414(19)
_cell_angle_beta                 68.429(3)
_cell_angle_gamma                87.206(2)
_cell_formula_units_Z            4
_cell_length_a                   16.5852(5)
_cell_length_b                   19.3538(4)
_cell_length_c                   21.8526(6)
_cell_measurement_reflns_used    40207
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      73.4840
_cell_measurement_theta_min      3.0160
_cell_volume                     6475.0(3)
_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      101(2)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega  -34.00   34.00   1.0000    1.0300
omega____ theta____ kappa____ phi______ frames
    -      -40.8413   37.0000  150.0000 68

  2 omega  -63.00  -36.00   1.0000    1.0300
omega____ theta____ kappa____ phi______ frames
    -      -40.8413   57.0000 -180.0000 27

  3 omega  -85.00   -3.00   1.0000    1.0300
omega____ theta____ kappa____ phi______ frames
    -      -40.8413  125.0000    0.0000 82

  4 omega  -48.00   24.00   1.0000    1.0300
omega____ theta____ kappa____ phi______ frames
    -      -40.8413   37.0000   30.0000 72

  5 omega -115.00  -11.00   1.0000    1.0300
omega____ theta____ kappa____ phi______ frames
    -      -40.8413  -57.0000 -120.0000 104

  6 omega  -92.00  -33.00   1.0000    1.0300
omega____ theta____ kappa____ phi______ frames
    -      -40.8413  125.0000 -180.0000 59

  7 omega   -6.00   27.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      -55.5000   15.0000 -120.0000 33

  8 omega  -38.00  -11.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      -55.5000   15.0000 -120.0000 27

  9 omega  110.00  178.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326   15.0000 -180.0000 68

 10 omega   35.00   93.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -45.0000 -150.0000 58

 11 omega   33.00   98.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -45.0000   90.0000 65

 12 omega   59.00  121.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326 -125.0000 -120.0000 62

 13 omega   32.00   89.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -45.0000  -60.0000 57

 14 omega   50.00  109.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -94.0000 -120.0000 59

 15 omega   31.00   97.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -94.0000  120.0000 66

 16 omega  139.00  166.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326   61.0000   60.0000 27

 17 omega   60.00   88.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -30.0000    0.0000 28

 18 omega   29.00   90.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -30.0000  150.0000 61

 19 omega   47.00  178.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326   15.0000  120.0000 131

 20 omega   23.00  109.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -94.0000  -30.0000 86

 21 omega   34.00  106.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -94.0000   60.0000 72

 22 omega -120.00   -7.00   1.0000    1.0300
omega____ theta____ kappa____ phi______ frames
    -      -40.8413  -77.0000  -90.0000 113

 23 omega -115.00  -11.00   1.0000    1.0300
omega____ theta____ kappa____ phi______ frames
    -      -40.8413  -57.0000  -30.0000 104

 24 omega -120.00   -7.00   1.0000    1.0300
omega____ theta____ kappa____ phi______ frames
    -      -40.8413  -77.0000   90.0000 113

 25 omega  -49.00   35.00   1.0000    1.0300
omega____ theta____ kappa____ phi______ frames
    -      -40.8413   37.0000   90.0000 84

 26 omega -120.00   -7.00   1.0000    1.0300
omega____ theta____ kappa____ phi______ frames
    -      -40.8413  -77.0000 -180.0000 113

 27 omega    1.00   83.00   1.0000    1.0300
omega____ theta____ kappa____ phi______ frames
    -       40.8413  -99.0000  -60.0000 82

 28 omega -134.00  -22.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -77.0000 -120.0000 112

 29 omega -134.00  -22.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -77.0000   30.0000 112

 30 omega -134.00  -22.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -77.0000  150.0000 112

 31 omega   77.00  178.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326   30.0000  -90.0000 101

 32 omega   73.00  178.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326   77.0000   60.0000 105

 33 omega   73.00  178.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326   77.0000    0.0000 105

 34 omega   23.00  109.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -94.0000    0.0000 86

 35 omega   79.00  178.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326   45.0000  -60.0000 99

 36 omega   77.00  178.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326   61.0000  120.0000 101

 37 omega   73.00  178.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326   77.0000 -120.0000 105

 38 omega   73.00  178.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326   77.0000 -180.0000 105

 39 omega   77.00  178.00   1.0000    4.1100
omega____ theta____ kappa____ phi______ frames
    -      107.0326   30.0000    0.0000 101

 40 omega   23.00   98.00   1.0000    1.0300
omega____ theta____ kappa____ phi______ frames
    -       40.8413 -125.0000 -120.0000 75
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0178728000
_diffrn_orient_matrix_UB_12      -0.0788048000
_diffrn_orient_matrix_UB_13      0.0116436000
_diffrn_orient_matrix_UB_21      0.0872788000
_diffrn_orient_matrix_UB_22      -0.0140139000
_diffrn_orient_matrix_UB_23      0.0092486000
_diffrn_orient_matrix_UB_31      -0.0451654000
_diffrn_orient_matrix_UB_32      0.0049099000
_diffrn_orient_matrix_UB_33      0.0748166000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            119292
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.92
_diffrn_reflns_theta_min         2.90
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.699
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.572
_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    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2691
_exptl_crystal_size_max          0.4682
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1614
_refine_ls_number_reflns         25669
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0833P)^2^+1.5520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1375
_reflns_number_gt                21196
_reflns_number_total             25669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01380_si_002.cif
_cod_data_source_block           complex1
_cod_original_formula_sum        'C63.50 H79.86 Cl0.14 Cu2 F3 N7 O7.43 S'
_cod_database_code               4346380
_chemical_oxdiff_formula         'C61 H70 Cu2 F3 N7 O5 S C2 H8 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, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F1B) = Uanis(F1A)
Uanis(C62B) = Uanis(C62A)
Uanis(F2B) = Uanis(F2A)
Uanis(F3B) = Uanis(F3A)
Uanis(O3B) = Uanis(O3A)
Uanis(O5B) = Uanis(O5A)
Uanis(O4B) = Uanis(O4A)
3. Same fragment restrains
{S1A, F1A, F2A, F3A, O3A, O4A, O5A, C62A}
as
{S1B, F1B, F2B, F3B, O3B, O4B, O5B, C62B}
4. Others
 Sof(S1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(O3B)=Sof(O4B)=Sof(O5B)=Sof(C62B)=
 Sof(Cl1)=Sof(Cl2)=Sof(C1X)=Sof(H1XA)=Sof(H1XB)=1-FVAR(1)
 Sof(S1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(C62A)=
 Sof(O1S)=Sof(H1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1X(H1XA,H1XB)
5.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), C49(H49), C50(H50), C51(H51),
  C52(H52), C53(H53), C57(H57), C58(H58), C59(H59), C60(H60), C4A(H4A),
 C6A(H6AA), C7A(H7A), C18A(H18A), C19A(H19A), C21A(H21A), C26A(H26A),
 C28A(H28A), C29A(H29A), C40A(H40A), C41A(H41A), C43A(H43A), C45A(H45A),
 C49A(H49A), C50A(H50A), C51A(H51A), C52A(H52A), C53A(H53A), C57A(H57A),
 C58A(H58A), C59A(H59A), C60A(H60A)
5.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), C46(H46A,H46B,
 H46C), C54(H54A,H54B,H54C), C61(H61A,H61B,H61C), C9A(H9AA,H9AB,H9AC),
 C10A(H10D,H10E,H10F), C11A(H11D,H11E,H11F), C13A(H13D,H13E,H13F), C14A(H14D,
 H14E,H14F), C15A(H15D,H15E,H15F), C22A(H22D,H22E,H22F), C31A(H31D,H31E,H31F),
 C32A(H32D,H32E,H32F), C33A(H33D,H33E,H33F), C35A(H35D,H35E,H35F), C36A(H36D,
 H36E,H36F), C37A(H37D,H37E,H37F), C44A(H44D,H44E,H44F), C46A(H46D,H46E,H46F),
 C54A(H54D,H54E,H54F), C61A(H61D,H61E,H61F), C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,
 H2SC), C3S(H3SA,H3SB,H3SC)
5.d Idealised tetrahedral OH refined as rotating group:
 O1S(H1S), O2S(H2S), O3S(H3S)
;
_olex2_submission_special_instructions 'No special instructions were received'