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_4345734
_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
'C65 H73 Cl2 Co N5 O10 P3 Ru2, C4 H10 O, 0.5(O2)'
_chemical_formula_sum            'C69 H85 Cl2 Co N5 O12 P3 Ru2'
_chemical_formula_weight         1601.30
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8979(3)
_cell_length_b                   19.1466(3)
_cell_length_c                   25.3158(3)
_cell_measurement_reflns_used    23331
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      71.6100
_cell_measurement_theta_min      4.1330
_cell_volume                     7221.2(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega   39.00   69.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000  -30.0000 30

  2 omega  -68.00   19.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 87

  3 omega   35.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   57.0000  150.0000 89

  4 omega   52.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   57.0000   90.0000 72

  5 omega   74.00  126.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000    0.0000 52

  6 omega  -14.00   76.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -57.0000    0.0000 90

  7 omega -112.00   -7.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  111.0000  -90.0000 105

  8 omega   40.00   72.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000    0.0000 32

  9 omega   82.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000 -150.0000 96

 10 omega   46.00   72.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000 -120.0000 26

 11 omega   37.00   72.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -90.0000 35

 12 omega   50.00   85.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  120.0000 35

 13 omega   38.00   70.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000   90.0000 32

 14 omega   37.00   72.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -60.0000 35

 15 omega   38.00   73.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -180.0000 35

 16 omega   38.00   69.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  150.0000 31

 17 omega   42.00   69.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000   60.0000 27

 18 omega   84.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000  120.0000 94

 19 omega   39.00   70.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -150.0000 31

 20 omega   44.00  112.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000  -90.0000 68

 21 omega  123.00  149.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000  -90.0000 26

 22 omega   38.00  142.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -93.0000  -13.8558 104

 23 omega   40.00  148.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -93.0000  115.2083 108
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42303
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.997
_diffrn_reflns_theta_min         4.146
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35
_diffrn_source_power             1.75
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.940
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 5121 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.033(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         12749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0337P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                12166
_reflns_number_total             12749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00281_si_003.cif
_cod_data_source_block           win36cult
_cod_database_code               4345734
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O1W(0.5) O1WA(0.5)
3.a Riding coordinates:
 O10(H10A,H10B)
3.b 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.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C32(H32), C33(H33), C37(H37),
 C38(H38), C42(H42), C43(H43), C47(H47), C48(H48), C52(H52), C53(H53), C55(H55),
  C56(H56), C62(H62), C63(H63), C65(H65), C66(H66), C72(H72), C73(H73),
 C75(H75), C76(H76), C82(H82), C83(H83), C85(H85), C86(H86)
3.d 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), C57(H57A,H57B,H57C), C67(H67A,
 H67B,H67C), C77(H77A,H77B,H77C), C87(H87A,H87B,H87C), C1S(H1SA,H1SB,H1SC),
 C5S(H5SA,H5SB,H5SC)
;
_shelx_res_checksum              87454
_shelx_hkl_checksum              1294
_olex2_submission_special_instructions 'No special instructions were received'