Construction of Alkyl-Substituted Pentaphosphido Ligands in the Coordination Sphere of Cobalt
Ziegler, Christoph G. P.; Maier, Thomas M.; Pelties, Stefan; Taube, Clemens; Hennersdorf, Felix; Ehlers, A.W.; Weigand, Jan J.; Wolf, Robert; Chemical Science  (2019) –; doi:10.1039/C8SC04745F

data_1550327
_publ_section_title
;
 Construction of Alkyl-Substituted Pentaphosphido Ligands in the
 Coordination Sphere of Cobalt
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04745F
_journal_year                    2019
_chemical_formula_moiety         'C63 H78 Cl Co Ga N4 P5, 2(C6 H5 F)'
_chemical_formula_sum            'C75 H88 Cl Co F2 Ga N4 P5'
_chemical_formula_weight         1402.44
_chemical_name_systematic        '[(MesBIAN)Co(? \h4:\h1 P5tBu)GaCl(nacnac)]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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     dual
_audit_creation_date             2018-10-18
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2018-10-18 deposited with the CCDC.
2018-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                89.008(2)
_cell_angle_beta                 77.087(2)
_cell_angle_gamma                78.673(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8741(3)
_cell_length_b                   12.4783(3)
_cell_length_c                   24.9702(6)
_cell_measurement_reflns_used    17670
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      74.0240
_cell_measurement_theta_min      3.8640
_cell_volume                     3534.62(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -66.00  28.00   1.00    2.50    --  -42.31  57.00-120.00   94
  2  \w    -68.00  19.00   1.00    2.50    --  -42.31  57.00  30.00   87
  3  \w   -112.00 -16.00   1.00    2.50    --  -42.31 -57.00  90.00   96
  4  \w      5.00  95.00   1.00    2.50    --   42.31-125.00   0.00   90
  5  \w     30.00  76.00   1.00   10.00    --  106.63 -94.00 -30.00   46
  6  \w     36.00  75.00   1.00   10.00    --  106.63 -45.00  90.00   39
  7  \w     93.00 131.00   1.00   10.00    --  106.63  45.00-180.00   38
  8  \w     32.00 105.00   1.00   10.00    --  106.63 -94.00   0.00   73
  9  \w     85.00 154.00   1.00   10.00    --  106.63  45.00  90.00   69
 10  \w     47.00  72.00   1.00   10.00    --  106.63 -45.00  60.00   25
 11  \w     97.00 145.00   1.00   10.00    --  106.63  15.00 -30.00   48
 12  \w     33.00 147.00   1.00   10.00    --  106.63 -15.00 -90.00  114
 13  \w     54.00 106.00   1.00   10.00    --  106.63 -94.00 120.00   52
 14  \w     56.00 122.00   1.00   10.00    --  106.63-125.00-120.00   66
 15  \w     32.00  68.00   1.00   10.00    --  106.63 -30.00 150.00   36
 16  \w     39.00  75.00   1.00   10.00    --  106.63 -45.00 -30.00   36
 17  \w     36.00  71.00   1.00   10.00    --  106.63-125.00 -30.00   35
 18  \w     92.00 118.00   1.00   10.00    --  106.63-125.00 -30.00   26
 19  \w     33.00  69.00   1.00   10.00    --  106.63 -30.00-180.00   36
 20  \w     42.00  67.00   1.00   10.00    --  106.63 -61.00  60.00   25
 21  \w    102.00 129.00   1.00   10.00    --  106.63 -61.00  60.00   27
 22  \w     62.00  93.00   1.00   10.00    --  106.63  15.00 -30.00   31
 23  \w     34.00 108.00   1.00   10.00    --  106.63 -94.00  60.00   74
 24  \w     49.00 115.00   1.00   10.00    --  106.63 -77.00-150.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0039365000
_diffrn_orient_matrix_UB_12      -0.0192556000
_diffrn_orient_matrix_UB_13      -0.0612225000
_diffrn_orient_matrix_UB_21      -0.0777205000
_diffrn_orient_matrix_UB_22      -0.0861453000
_diffrn_orient_matrix_UB_23      0.0155869000
_diffrn_orient_matrix_UB_31      -0.1112708000
_diffrn_orient_matrix_UB_32      0.0898570000
_diffrn_orient_matrix_UB_33      0.0042927000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            28770
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.207
_diffrn_reflns_theta_min         3.614
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.115
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.331
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.18b (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             1468
_exptl_crystal_recrystallization_method 'slow evaporation form fluorobenzene'
_exptl_crystal_size_max          0.402
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.197
_refine_diff_density_max         1.854
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         13997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0731P)^2^+1.8771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13408
_reflns_number_total             13997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04745f2.cif
_cod_data_source_block           zic111
_cod_original_cell_volume        3534.63(15)
_cod_database_code               1550327
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C75 H88 Cl Co F2 Ga N4 P5 '
_chemical_oxdiff_usercomment     fluorobenzene
_shelx_estimated_absorpt_t_max   0.498
_shelx_estimated_absorpt_t_min   0.289
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H85)=Sof(F90)=1-FVAR(1)
 Sof(H87)=Sof(F89)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C67(H67), C64(H64), C70(H70), C73(H73)
3.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C22(H22), C21(H21), C20(H20), C17(H17), C18(H18), C40(H40),
 C53(H53), C60(H60), C28(H28), C30(H30), C38(H38), C61(H61), C49(H49), C62(H62),
  C47(H47), C48(H48), C77(H77), C78(H78), C85(H85), C88(H88), C84(H84),
 C81(H81), C83(H83), C87(H87), C80(H80), C79(H79), C86(H86)
3.c Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C43(H43A,H43B,H43C), C69(H69A,H69B,H69C), C57(H57A,H57B,
 H57C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C72(H72A,H72B,H72C), C68(H68A,
 H68B,H68C), C75(H75A,H75B,H75C), C10(H10A,H10B,H10C), C34(H34A,H34B,H34C),
 C71(H71A,H71B,H71C), C74(H74A,H74B,H74C), C44(H44A,H44B,H44C), C66(H66A,H66B,
 H66C), C65(H65A,H65B,H65C), C32(H32A,H32B,H32C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C)
;
_shelx_res_checksum              96281
_olex2_date_sample_data_collection 2018-05-09
_olex2_submission_original_sample_id zic111
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.674
_oxdiff_exptl_absorpt_empirical_full_min 0.588