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_1550319
_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         'C38 H46 Co N2 P5, C3 H7'
_chemical_formula_sum            'C41 H53 Co N2 P5'
_chemical_formula_weight         787.63
_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                71.013(4)
_cell_angle_beta                 69.473(5)
_cell_angle_gamma                70.661(4)
_cell_formula_units_Z            2
_cell_length_a                   11.5086(6)
_cell_length_b                   12.6623(6)
_cell_length_c                   16.1055(8)
_cell_measurement_reflns_used    6952
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.9410
_cell_measurement_theta_min      4.1680
_cell_volume                     2014.97(19)
_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 10.3546
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.960
_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    -71.00  31.00   1.00    2.75    --  -42.46  57.00   0.00  102
  2  \w    -66.00  32.00   1.00    2.75    --  -42.46  37.00 150.00   98
  3  \w     55.00  87.00   1.00    2.75    --   42.46-125.00 150.00   32
  4  \w     26.00  97.00   1.00   11.00    --  106.35 -94.00  90.00   71
  5  \w     54.00 117.00   1.00   11.00    --  106.35-125.00   0.00   63
  6  \w     82.00 120.00   1.00   11.00    --  106.35-125.00-150.00   38
  7  \w     65.00 137.00   1.00   11.00    --  106.35 -77.00-180.00   72
  8  \w    118.00 158.00   1.00   11.00    --  106.35  45.00-180.00   40
  9  \w     92.00 145.00   1.00   11.00    --  106.35  77.00 -90.00   53
 10  \w     74.00 141.00   1.00   11.00    --  106.35  77.00  30.00   67
 11  \w     93.00 155.00   1.00   11.00    --  106.35  45.00 150.00   62
 12  \w     31.00  64.00   1.00   11.00    --  106.35 -30.00 -90.00   33
 13  \w     34.00  64.00   1.00   11.00    --  106.35 -45.00 -30.00   30
 14  \w     29.00 109.00   1.00   11.00    --  106.35 -94.00   0.00   80
 15  \w     34.00 135.00   1.00   11.00    --  106.35 -61.00  90.00  101
 16  \w     76.00 158.00   1.00   11.00    --  106.35  77.00-120.00   82
 17  \w     31.00  59.00   1.00   11.00    --  106.35 -30.00-180.00   28
 18  \w   -108.00 -22.00   1.00    2.75    --  -42.46 -57.00-150.00   86
;
_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      -0.0905815000
_diffrn_orient_matrix_UB_12      0.0960653000
_diffrn_orient_matrix_UB_13      0.0480955000
_diffrn_orient_matrix_UB_21      0.1135313000
_diffrn_orient_matrix_UB_22      0.0141933000
_diffrn_orient_matrix_UB_23      0.0215238000
_diffrn_orient_matrix_UB_31      0.0253581000
_diffrn_orient_matrix_UB_32      0.0904608000
_diffrn_orient_matrix_UB_33      -0.0909710000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13999
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.089
_diffrn_reflns_theta_min         3.808
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.446
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_correction_T_min  0.354
_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            'clear blackish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             830
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.158
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         7873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0544
_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^)+(0.1137P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1501
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7490
_reflns_number_total             7873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04745f2.cif
_cod_data_source_block           3b_[MesBIAN)Co(P5)(tBu)2]
_cod_original_cell_volume        2015.0(2)
_cod_database_code               1550319
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C41 H53 N2 P5 Co1 '
_shelx_estimated_absorpt_t_max   0.480
_shelx_estimated_absorpt_t_min   0.245
_reflns_odcompleteness_completeness 99.44
_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 Secondary CH2 refined with riding coordinates:
 C015(H01,H), C01A(H0AA,HA)
2.b Aromatic/amide H refined with riding coordinates:
 C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00R(H00R), C00S(H00S), C00T(H00T), C00Z(H00Z)
2.c Idealised Me refined as rotating group:
 C00V(H00A,H00B,H00C), C00Y(H00D,H00E,H00F), C010(H01A,H01B,H01C), C011(H01D,
 H01E,H01F), C012(H01G,H01H,H01I), C014(H01J,H01K,H01L), C016(H01M,H01N,H01O),
 C017(H01P,H01Q,H01R), C018(H01S,H01T,H01U), C019(H01V,H01W,H01X), C01B(H1AA,HB,
 HC), C01C(H01Y,HD,HE), C01D(H01Z,HF,HG)
;
_shelx_res_checksum              28049
_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 1.821
_oxdiff_exptl_absorpt_empirical_full_min 0.601