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_4346379
_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         'C44 H57 N3 O2'
_chemical_formula_sum            'C44 H57 N3 O2'
_chemical_formula_weight         659.93
_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             2014-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                101.685(3)
_cell_angle_beta                 109.567(3)
_cell_angle_gamma                95.189(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9973(3)
_cell_length_b                   14.7313(5)
_cell_length_c                   14.8047(5)
_cell_measurement_reflns_used    13776
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.6240
_cell_measurement_theta_min      3.2660
_cell_volume                     1982.03(12)
_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      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega -120.00   -7.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.9351  -77.0000 -180.0000 113

  2 omega  -41.00   19.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.9351   37.0000  -60.0000 60

  3 omega   36.00   92.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       40.9351 -125.0000   30.0000 56

  4 omega  -31.00   70.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       40.9351  -57.0000   30.0000 101

  5 omega -130.00  -95.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -94.0000 -180.0000 35

  6 omega   24.00  109.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -94.0000   90.0000 85

  7 omega   79.00  177.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   30.0000 -120.0000 98

  8 omega   31.00   61.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -30.0000   60.0000 30

  9 omega   86.00  115.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326 -125.0000 -180.0000 29

 10 omega   84.00  109.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -94.0000 -180.0000 25

 11 omega   36.00   76.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -45.0000  -30.0000 40

 12 omega   39.00   89.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -30.0000 -180.0000 50

 13 omega  151.00  176.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  125.0000  150.0000 25

 14 omega   33.00  118.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326 -125.0000   30.0000 85

 15 omega   53.00   79.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -30.0000  -30.0000 26

 16 omega   84.00  109.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -94.0000  -90.0000 25

 17 omega   40.00   84.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -45.0000   90.0000 44

 18 omega   78.00  173.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   30.0000  -30.0000 95

 19 omega   98.00  124.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  125.0000  150.0000 26

 20 omega   28.00  138.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -77.0000 -180.0000 110

 21 omega -115.00  -11.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.9351  -57.0000   60.0000 104

 22 omega -115.00  -11.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.9351  -57.0000 -120.0000 104

 23 omega  -96.00   -2.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.9351  125.0000  150.0000 94

 24 omega -115.00  -11.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.9351  -57.0000  -30.0000 104

 25 omega -134.00  -22.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -77.0000  150.0000 112

 26 omega -134.00  -22.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -77.0000   60.0000 112

 27 omega -134.00  -22.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -77.0000  -30.0000 112

 28 omega -134.00  -22.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -77.0000 -120.0000 112

 29 omega   73.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   77.0000  150.0000 105

 30 omega   77.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   61.0000    0.0000 101

 31 omega   28.00  141.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326  -77.0000 -180.0000 113

 32 omega   77.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   30.0000  120.0000 101

 33 omega   77.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   61.0000  -90.0000 101

 34 omega   73.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   77.0000  120.0000 105

 35 omega   73.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   77.0000 -150.0000 105

 36 omega   77.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0326   61.0000   60.0000 101

 37 omega -120.00   -7.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.9351  -77.0000   30.0000 113

 38 omega   15.00  117.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       40.9351   37.0000  120.0000 102

 39 omega    1.00   83.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       40.9351  -99.0000   30.0000 82
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0450219000
_diffrn_orient_matrix_UB_12      -0.0515424000
_diffrn_orient_matrix_UB_13      -0.0838207000
_diffrn_orient_matrix_UB_21      -0.1338284000
_diffrn_orient_matrix_UB_22      0.0203633000
_diffrn_orient_matrix_UB_23      -0.0771927000
_diffrn_orient_matrix_UB_31      0.0872936000
_diffrn_orient_matrix_UB_32      0.0931594000
_diffrn_orient_matrix_UB_33      0.0034082000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15488
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.75
_diffrn_reflns_theta_min         3.11
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90872
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         15488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0757P)^2^+0.7255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                13397
_reflns_number_total             15488
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01380_si_002.cif
_cod_data_source_block           H3LN3O2
_cod_original_cell_volume        1982.02(12)
_cod_database_code               4346379
_chemical_oxdiff_formula         'Ni2 O2 N5 C66 H70 Cl2'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C4(H4), C6(H6), C7(H7), C18(H18), C19(H19), C21(H21), C26(H26),
 C28(H28), C29(H29), C40(H40), C41(H41), C43(H43)
2.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)
;
_olex2_submission_special_instructions 'No special instructions were received'