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_1550325
_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         'C67 H89 Co Ga K N4 O4 P4'
_chemical_formula_sum            'C67 H89 Co Ga K N4 O4 P4'
_chemical_formula_weight         1306.05
_chemical_properties_physical    Air-sensitive,Moisture-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     direct
_audit_creation_date             2018-08-13
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2018-08-13 deposited with the CCDC.
2018-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                94.7947(16)
_cell_angle_beta                 103.1479(16)
_cell_angle_gamma                98.1715(18)
_cell_formula_units_Z            2
_cell_length_a                   15.4512(3)
_cell_length_b                   16.1163(4)
_cell_length_c                   16.5636(3)
_cell_measurement_reflns_used    28113
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      76.4430
_cell_measurement_theta_min      4.3480
_cell_volume                     3946.85(15)
_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    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
  1 omega  -74.00   38.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064   77.0000  -30.0000 112

  2 omega  -74.00   38.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064   77.0000   90.0000 112

  3 omega  -74.00   38.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064   77.0000 -150.0000 112

  4 omega   83.00  158.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  150.0000 75

  5 omega   37.00  117.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -117.0000  116.0000 80

  6 omega   35.00  116.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -150.0000 81

  7 omega   83.00  158.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  120.0000 75

  8 omega   24.00  158.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000    0.0000  120.0000 134

  9 omega   29.00  109.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000   30.0000 80

 10 omega   34.00  147.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000   60.0000 113

 11 omega   38.00   77.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -60.0000 39

 12 omega   35.00  116.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  -60.0000 81

 13 omega   35.00   69.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   30.0000 34

 14 omega   52.00  158.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000    0.0000 106

 15 omega   35.00   69.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  150.0000 34

 16 omega   79.00  158.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   30.0000 79

 17 omega   29.00  109.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000 -120.0000 80

 18 omega   34.00  147.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  -60.0000 113

 19 omega -119.00   -7.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064  -77.0000 -120.0000 112

 20 omega -119.00   -7.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064  -77.0000    0.0000 112

 21 omega -119.00   -7.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064  -77.0000  120.0000 112

 22 omega    2.00   28.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -       40.7064   92.0000  100.9283 26

 23 omega   35.00   69.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   60.0000 34

 24 omega   83.00  158.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -180.0000 75

 25 omega   82.00  158.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000 -120.0000 76

 26 omega   83.00  158.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   90.0000 75

 27 omega   79.00  158.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -120.0000 79

 28 omega   35.00   69.00   1.0000    8.4000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   90.0000 34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0532389000
_diffrn_orient_matrix_UB_12      -0.0358621000
_diffrn_orient_matrix_UB_13      -0.0894551000
_diffrn_orient_matrix_UB_21      -0.0841630000
_diffrn_orient_matrix_UB_22      -0.0273324000
_diffrn_orient_matrix_UB_23      0.0326094000
_diffrn_orient_matrix_UB_31      -0.0293785000
_diffrn_orient_matrix_UB_32      0.0861952000
_diffrn_orient_matrix_UB_33      -0.0138202000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50128
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         76.512
_diffrn_reflns_theta_min         3.536
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.623
_exptl_absorpt_correction_T_max  0.675
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_type   gaussian
_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)
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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DME/n-hexane'
_exptl_crystal_size_max          0.3316
_exptl_crystal_size_mid          0.1837
_exptl_crystal_size_min          0.1439
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         16206
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0641P)^2^+1.9634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15529
_reflns_number_total             16206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04745f2.cif
_cod_data_source_block           2_[K(dme)2][(MesBIANCo)P4(GaDippNACNAC)]
_cod_original_cell_volume        3946.83(14)
_cod_database_code               1550325
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C67 H89 Ga P4 Co N4 K O5'
_reflns_odcompleteness_completeness 99.91
_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
2.a Ternary CH refined with riding coordinates:
 C42(H42), C45(H45), C54(H54), C57(H57)
2.b Secondary CH2 refined with riding coordinates:
 C61(H61a,H61b), C62(H62a,H62b), C65(H65a,H65b), C66(H66a,H66b)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C15(H15), C17(H17),
 C24(H24), C26(H26), C32(H32), C38(H38), C39(H39), C40(H40), C50(H50), C51(H51),
  C52(H52)
2.d Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C21(H21a,H21b,H21c), C28(H28a,H28b,
 H28c), C29(H29a,H29b,H29c), C30(H30a,H30b,H30c), C34(H34a,H34b,H34c), C35(H35a,
 H35b,H35c), C43(H43a,H43b,H43c), C44(H44a,H44b,H44c), C46(H46a,H46b,H46c),
 C47(H47a,H47b,H47c), C55(H55a,H55b,H55c), C56(H56a,H56b,H56c), C58(H58a,H58b,
 H58c), C59(H59a,H59b,H59c), C60(H60a,H60b,H60c), C63(H63a,H63b,H63c), C64(H64a,
 H64b,H64c), C67(H67a,H67b,H67c)
;
_shelx_res_checksum              29065
_shelx_fab_checksum              99706
_olex2_submission_special_instructions 'No special instructions were received'