Heterobimetallic Nitrido Complexes of Group 8 Metalloporphyrins
Cheung, Wai-Man; Chiu, Wai-Hang; de Vere-Tucker, Matthew; Sung, Herman H.-Y.; Williams, Ian D.; Leung, Wa-Hung; Inorganic Chemistry  (2017) –; doi:10.1021/acs.inorgchem.7b00281

data_4345735
_publ_section_title
;
 Heterobimetallic Nitrido Complexes of Group 8 Metalloporphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.7b00281
_journal_year                    2017
_chemical_formula_moiety         'C66 H68 Cl2 Co Fe N6 O9 P3 Ru, C4 H10 O'
_chemical_formula_sum            'C70 H78 Cl2 Co Fe N6 O10 P3 Ru'
_chemical_formula_weight         1543.04
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                85.814(3)
_cell_angle_beta                 81.328(3)
_cell_angle_gamma                79.174(3)
_cell_formula_units_Z            2
_cell_length_a                   13.0815(5)
_cell_length_b                   13.5417(5)
_cell_length_c                   20.0834(8)
_cell_measurement_reflns_used    7821
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.2840
_cell_measurement_theta_min      4.5720
_cell_volume                     3450.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega   41.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000   30.0000 74

  2 omega  -64.00   33.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6953   57.0000   60.0000 97

  3 omega   34.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6953  -99.0000   90.0000 49

  4 omega   36.00  139.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -61.0000   30.0000 103

  5 omega   53.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   15.0000  120.0000 123

  6 omega  103.00  175.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  111.0000    0.0000 72

  7 omega   93.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   45.0000 -180.0000 85

  8 omega   73.00  149.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  178.0000   30.0000 76

  9 omega   34.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000  -90.0000 52

 10 omega   51.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000 -180.0000 39

 11 omega   39.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000 -150.0000 75

 12 omega -109.00  -13.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6953  -57.0000  -90.0000 96

 13 omega -115.00  -11.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6953  -57.0000 -180.0000 104
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0622154000
_diffrn_orient_matrix_UB_12      0.0405983000
_diffrn_orient_matrix_UB_13      0.0479419000
_diffrn_orient_matrix_UB_21      -0.0805727000
_diffrn_orient_matrix_UB_22      -0.0236714000
_diffrn_orient_matrix_UB_23      0.0604860000
_diffrn_orient_matrix_UB_31      0.0655775000
_diffrn_orient_matrix_UB_32      -0.1059979000
_diffrn_orient_matrix_UB_33      0.0087637000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19603
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.999
_diffrn_reflns_theta_min         3.919
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    7.154
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         12128
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1163
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9860
_reflns_number_total             12128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00281_si_003.cif
_cod_data_source_block           wai178cult
_cod_database_code               4345735
_chemical_oxdiff_formula         'Fe Ru N4 ph8 Co Et6 O9 P3 Cl2'
_reflns_odcompleteness_completeness 98.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of
0.002
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,
 H19B), C21(H21A,H21B), C2S(H2SA,H2SB), C4S(H4SA,H4SB)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C32(H32), C33(H33), C37(H37), C38(H38), C42(H42), C43(H43), C47(H47),
  C48(H48), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62),
 C63(H63), C64(H64), C65(H65), C66(H66), C72(H72), C73(H73), C74(H74), C75(H75),
  C76(H76), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C1S(H1SA,H1SB,H1SC), C5S(H5SA,
 H5SB,H5SC)
;
_shelx_res_checksum              53279
_shelx_hkl_checksum              53729
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-01-25
_olex2_submission_special_instructions 'No special instructions were received'