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_1550322
_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, C4 H7.16 O'
_chemical_formula_sum            'C69 H89.27 Co Ga N4 O P5'
_chemical_formula_weight         1274.21
_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                97.670(2)
_cell_angle_beta                 101.165(2)
_cell_angle_gamma                94.952(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5761(4)
_cell_length_b                   16.9742(4)
_cell_length_c                   17.4872(4)
_cell_measurement_reflns_used    13515
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.8280
_cell_measurement_theta_min      4.1890
_cell_volume                     3605.33(17)
_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    'ShelXT (Sheldrick, 2015)'
_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 0.980
_diffrn_measured_fraction_theta_max 0.935
_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      -0.0076929000
_diffrn_orient_matrix_UB_12      -0.0831611000
_diffrn_orient_matrix_UB_13      0.0259942000
_diffrn_orient_matrix_UB_21      0.1236927000
_diffrn_orient_matrix_UB_22      -0.0011241000
_diffrn_orient_matrix_UB_23      0.0060424000
_diffrn_orient_matrix_UB_31      0.0210216000
_diffrn_orient_matrix_UB_32      0.0397825000
_diffrn_orient_matrix_UB_33      0.0868680000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21456
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.972
_diffrn_reflns_theta_min         3.606
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.620
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69538
_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    1.174
_exptl_crystal_description       plate
_exptl_crystal_F_000             1345
_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         1.641
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         13684
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0647
_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^)+(0.1370P)^2^+1.1744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1798
_refine_ls_wR_factor_ref         0.1832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12927
_reflns_number_total             13684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04745f2.cif
_cod_data_source_block
4_[MesBIAN)Co(P5)(iPr)2Ga(Dippnacnac)]_multicrystal1
_cod_database_code               1550322
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-C2 \\sim C3-C1
 with sigma of 0.001
 O3-C3 \\sim O3-C4
 with sigma of 0.001
 O3-C4 \\sim O5-C0AA \\sim O5-C3 \\sim O3-C3
 with sigma of 0.001
 C2-C1 \\sim C3-C1 \\sim C2-C0AA \\sim C4-C2
 with sigma of 0.001
 C4-C1 \\sim C3-C2
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O5)
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(O5)
Uanis(C0AA) = Uanis(C2) = Uanis(C4) = Uanis(C1) = Uanis(C3)
4. Others
 Sof(H2BD)=Sof(H2BE)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(O3)=1-FVAR(1)
 Sof(H2AB)=Sof(H2AC)=Sof(H3A)=Sof(H3B)=Sof(O5)=Sof(C0AA)=Sof(H0AB)=Sof(H0AC)=
 FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C010(H010), C013(H013), C014(H014), C01G(H01L), C01T(H3AA), C021(H021)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2BD,H2BE), C2(H2AB,H2AC), C3(H3A,H3B), C4(H4A,H4B),
 C0AA(H0AB,H0AC)
5.c Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00S(H00S), C00T(H00T), C00V(H00V), C00X(H00X), C012(H012),
 C015(H015), C017(H017), C019(H019), C01A(H01D), C01C(H01H), C01J(H01S),
 C01K(H01T), C01L(H01U), C01O(H01Z), C01Q(H0AA), C01X(H7AA)
5.d Idealised Me refined as rotating group:
 C00W(H00A,H00B,H00C), C011(H01A,H01B,H01C), C01B(H01E,H01F,H01G), C01F(H01I,
 H01J,H01K), C01H(H01M,H01N,H01O), C01I(H01P,H01Q,H01R), C01M(H01V,H01W,H01X),
 C01N(H01Y,H,HA), C01P(H01,HB,HC), C01R(H1AA,HD,HE), C01S(H2AA,HF,HG),
 C01U(H4AA,HH,HI), C01V(H5AA,HJ,HK), C01W(H6AA,HL,HM), C01Y(H8AA,HN,HO),
 C01Z(H9AA,HP,HQ), C020(H02A,H02B,H02C), C022(H02D,H02E,H02F), C023(H02G,H02H,
 H02I), C024(H02J,H02K,H02L)
;
_shelx_res_checksum              97479
_shelx_fab_checksum              96176
_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 6.028
_oxdiff_exptl_absorpt_empirical_full_min 0.272