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_1550320
_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         'C42 H50 Co N2 P5, C3 H7'
_chemical_formula_sum            'C45 H57 Co N2 P5'
_chemical_formula_weight         839.70
_chemical_name_systematic        '[MesBIANCoP5Cy2]'
_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     dual
_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                68.191(5)
_cell_angle_beta                 88.775(4)
_cell_angle_gamma                72.802(4)
_cell_formula_units_Z            2
_cell_length_a                   11.0975(4)
_cell_length_b                   12.9085(8)
_cell_length_c                   16.7384(9)
_cell_measurement_reflns_used    8063
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.5950
_cell_measurement_theta_min      3.8440
_cell_volume                     2116.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.958
_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     14.00 115.00   1.00   10.00    --   42.25  57.00 -60.00  101
  2  \w    -20.00  83.00   1.00   10.00    --   42.25 -99.00  60.00  103
  3  \w    -30.00  70.00   1.00   10.00    --   42.25 -57.00 150.00  100
  4  \w     33.00  77.00   1.00   40.00    --  106.43 -45.00 120.00   44
  5  \w     24.00 109.00   1.00   40.00    --  106.43 -94.00 -90.00   85
  6  \w     30.00 139.00   1.00   40.00    --  106.43 -77.00  90.00  109
  7  \w     25.00 158.00   1.00   40.00    --  106.43 -15.00-150.00  133
  8  \w     24.00 109.00   1.00   40.00    --  106.43 -94.00 -30.00   85
  9  \w     30.00  69.00   1.00   40.00    --  106.43 -30.00  30.00   39
 10  \w     33.00  77.00   1.00   40.00    --  106.43 -45.00   0.00   44
 11  \w     33.00 121.00   1.00   40.00    --  106.43-125.00 -90.00   88
 12  \w     24.00 109.00   1.00   40.00    --  106.43 -94.00  30.00   85
 13  \w     78.00 158.00   1.00   40.00    --  106.43  30.00-120.00   80
 14  \w     78.00 158.00   1.00   40.00    --  106.43  30.00 150.00   80
 15  \w     14.00 115.00   1.00   10.00    --   42.25  57.00  90.00  101
 16  \w     10.00 118.00   1.00   10.00    --   42.25  77.00   0.00  108
 17  \w     14.00 115.00   1.00   10.00    --   42.25  57.00-180.00  101
 18  \w     54.00  83.00   1.00   40.00    --  106.43  15.00  60.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0304408000
_diffrn_orient_matrix_UB_12      -0.0831984000
_diffrn_orient_matrix_UB_13      0.0856686000
_diffrn_orient_matrix_UB_21      0.0015460000
_diffrn_orient_matrix_UB_22      0.0870206000
_diffrn_orient_matrix_UB_23      0.0424868000
_diffrn_orient_matrix_UB_31      -0.1428307000
_diffrn_orient_matrix_UB_32      0.0615297000
_diffrn_orient_matrix_UB_33      -0.0279605000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19056
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.050
_diffrn_reflns_theta_min         3.839
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.220
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       plate
_exptl_crystal_F_000             886
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+4.2914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6914
_reflns_number_total             8231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04745f2.cif
_cod_data_source_block           3c_[MesBIAN)Co(P5)(Cy)2]
_cod_database_code               1550320
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C45 H57 Co N2 P5 '
_reflns_odcompleteness_completeness 99.14
_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:
 C00F(H00F), C00W(H00W)
2.b Secondary CH2 refined with riding coordinates:
 C00Q(H00D,H00E), C00T(H00G,H00H), C00Y(H00I,H00K), C010(H01A,H01B), C011(H01C,
 H01D), C014(H01E,H01F), C017(H01J,H01K), C018(H01L,H01M), C01B(H01T,H01U),
 C01D(H01Y,H), C01E(H01,HA), C01F(H0AA,HB)
2.c Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00M(H00M), C00N(H00N), C00P(H00P), C00R(H00R), C00U(H00U),
 C00V(H00V), C00Z(H00Z), C013(H013), C016(H016)
2.d Idealised Me refined as rotating group:
 C00O(H00A,H00B,H00C), C015(H01G,H01H,H01I), C019(H01N,H01O,H01P), C01A(H01Q,
 H01R,H01S), C01C(H01V,H01W,H01X), C01G(H01Z,HC,HD), C01H(H1AA,HE,HF)
;
_shelx_res_checksum              61061
_olex2_submission_original_sample_id zic098
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.239
_oxdiff_exptl_absorpt_empirical_full_min 0.553