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_1550326
_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         'C65 H83 Co Ga N4 P5, C3 H7'
_chemical_formula_sum            'C68 H90 Co Ga N4 P5'
_chemical_formula_weight         1246.93
_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             2018-05-22
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-08-13 deposited with the CCDC.
2018-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                99.614(4)
_cell_angle_beta                 94.655(4)
_cell_angle_gamma                102.639(4)
_cell_formula_units_Z            2
_cell_length_a                   12.0763(7)
_cell_length_b                   12.7169(7)
_cell_length_c                   21.8615(9)
_cell_measurement_reflns_used    6277
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.7510
_cell_measurement_theta_min      12.1630
_cell_volume                     3205.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (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    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.920
_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  25.00   0.50   10.00    --  -44.94  57.00-180.00  182
  2  \w     15.00 116.00   0.50   10.00    --   44.94  77.00  30.00  202
  3  \w    -20.00  75.00   0.50   10.00    --   44.94 -99.00 -60.00  190
  4  \w     61.00 129.00   0.50   40.00    --  104.50 -45.00-180.00  136
  5  \w     34.00 135.00   0.50   40.00    --  104.50 -15.00   0.00  202
  6  \w     29.00 109.00   0.50   40.00    --  104.50 -94.00-120.00  160
  7  \w     38.00 114.00   0.50   40.00    --  104.50 -45.00  90.00  152
  8  \w     40.00 131.00   0.50   40.00    --  104.50 -61.00 -60.00  182
  9  \w     45.00 121.00   0.50   40.00    --  104.50-125.00 150.00  152
 10  \w     66.00 168.00   0.50   40.00    --  104.50  15.00  30.00  204
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0068680000
_diffrn_orient_matrix_UB_12      0.0219870000
_diffrn_orient_matrix_UB_13      0.0718353000
_diffrn_orient_matrix_UB_21      0.1277691000
_diffrn_orient_matrix_UB_22      -0.0008631000
_diffrn_orient_matrix_UB_23      0.0049167000
_diffrn_orient_matrix_UB_31      0.0313031000
_diffrn_orient_matrix_UB_32      0.1245257000
_diffrn_orient_matrix_UB_33      0.0012439000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18878
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.940
_diffrn_reflns_theta_min         3.628
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.046
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
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    1.292
_exptl_crystal_description       plate
_exptl_crystal_F_000             1318
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.155
_refine_diff_density_max         1.161
_refine_diff_density_min         -1.436
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         11950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0717
_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^)+(0.1402P)^2^+0.6385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1887
_refine_ls_wR_factor_ref         0.2019
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10368
_reflns_number_total             11950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04745f2.cif
_cod_data_source_block
4_[MesBIAN)Co(P5)(iPr)2Ga(Dippnacnac)]_multicrystal2
_cod_database_code               1550326
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C69  O1 H87 N2 P5 Co1 Ga1'
_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:
 C00Q(H00Q), C01F(H01L), C3(H3), C01O(H01), C4(H4), C01X(H7AA)
2.b Secondary CH2 refined with riding coordinates:
 C023(H02P,H02Q), C027(H02U,H02V)
2.c Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00P(H00P), C00T(H00T), C00W(H00W), C00Z(H00Z), C010(H010),
 C012(H012), C013(H013), C014(H014), C015(H015), C01A(H01G), C01E(H01K),
 C01G(H01M), C01I(H01Q), C01M(H01Z), C01P(H0AA), C01U(H5AA)
2.d Idealised Me refined as rotating group:
 C00Y(H00A,H00B,H00C), C016(H01A,H01B,H01C), C019(H01D,H01E,H01F), C01B(H01H,
 H01I,H01J), C01H(H01N,H01O,H01P), C01J(H01R,H01S,H01T), C01K(H01U,H01V,H01W),
 C01L(H01X,H01Y,H), C01Q(H1AA,HA,HB), C01R(H2AA,HC,HD), C01S(H3AA,HE,HF),
 C01T(H4AA,HG,HH), C01V(H6AA,HI,HJ), C01Y(H8AA,HK,HL), C01Z(H9AA,HM,HN),
 C020(H02A,H02B,H02C), C021(H02D,H02E,H02F), C022(H02G,H02H,H02I), C024(H02J,
 H02K,H02L), C025(H02M,H02N,H02O), C026(H02R,H02S,H02T)
;
_olex2_submission_original_sample_id zic049
_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 4.716
_oxdiff_exptl_absorpt_empirical_full_min 0.414