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_1550318
_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         'C36 H42 Co N2 P5, 0.5(C6 H14)'
_chemical_formula_sum            'C39 H49 Co N2 P5'
_chemical_formula_weight         759.58
_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             2018-04-26
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2018-08-13 deposited with the CCDC.
2018-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                84.114(5)
_cell_angle_beta                 82.677(5)
_cell_angle_gamma                80.838(6)
_cell_formula_units_Z            2
_cell_length_a                   8.2950(6)
_cell_length_b                   10.3193(6)
_cell_length_c                   23.1847(14)
_cell_measurement_reflns_used    4504
_cell_measurement_temperature    122.96(18)
_cell_measurement_theta_max      73.3420
_cell_measurement_theta_min      4.3770
_cell_volume                     1936.4(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      122.96(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.944
_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   -113.00 -18.00   1.00   15.00    --  -43.73 -57.00 -90.00   95
  2  \w    -69.00  26.00   1.00   15.00    --  -43.73  57.00  60.00   95
  3  \w      3.00  81.00   1.00   15.00    --   43.73-125.00-150.00   78
  4  \w     30.00 133.00   1.00   25.00    --  104.50 -77.00   0.00  103
  5  \w    124.00 151.00   1.00   25.00    --  104.50  61.00 -30.00   27
  6  \w     35.00 120.00   1.00   25.00    --  104.50-125.00-150.00   85
  7  \w     79.00 108.00   1.00   25.00    --  104.50  61.00 -30.00   29
  8  \w     28.00 109.00   1.00   25.00    --  104.50 -94.00 -60.00   81
  9  \w     83.00 165.00   1.00   25.00    --  104.50  77.00  60.00   82
 10  \w     80.00 159.00   1.00   25.00    --  104.50  77.00-180.00   79
 11  \w     86.00 174.00   1.00   25.00    --  104.50  61.00 120.00   88
 12  \w     92.00 177.00   1.00   25.00    --  104.50 125.00   0.00   85
;
_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      0.0795584000
_diffrn_orient_matrix_UB_12      -0.0183646000
_diffrn_orient_matrix_UB_13      0.0573770000
_diffrn_orient_matrix_UB_21      -0.1523744000
_diffrn_orient_matrix_UB_22      0.0836229000
_diffrn_orient_matrix_UB_23      0.0298516000
_diffrn_orient_matrix_UB_31      -0.0793816000
_diffrn_orient_matrix_UB_32      -0.1252986000
_diffrn_orient_matrix_UB_33      0.0183524000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            11921
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.694
_diffrn_reflns_theta_min         3.858
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.648
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.531
_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            'light violet'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       plate
_exptl_crystal_F_000             798
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.037
_refine_diff_density_max         2.010
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         7390
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0793
_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^)+(0.1218P)^2^+4.3303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2044
_refine_ls_wR_factor_ref         0.2164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6221
_reflns_number_total             7390
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04745f2.cif
_cod_data_source_block           3a_[MesBIAN)Co(P5)(iPr)2]
_cod_database_code               1550318
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C35 H43 Co P5 N2'
_reflns_odcompleteness_completeness 98.93
_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. Uiso/Uaniso restraints and constraints
C5AA \\sim C4AA \\sim C3AA \\sim C2AA \\sim C1AA \\sim C0AA: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C5AA) = Uanis(C4AA) = Uanis(C3AA) = Uanis(C2AA) = Uanis(C1AA) =
Uanis(C0AA)
3. Others
 Fixed Sof: C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5) C1AA(0.5) H1AA(0.5)
 H1AB(0.5) C2AA(0.5) H2AA(0.5) H2AB(0.5) C3AA(0.5) H3AA(0.5) H3AB(0.5)
 C4AA(0.5) H4AA(0.5) H4AB(0.5) C5AA(0.5) H5AA(0.5) H5AB(0.5) H5AC(0.5)
4.a Free rotating group:
 C0AA(C1AA,C2AA,C3AA,C4AA,C5AA)
4.b Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
4.c Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB), C2AA(H2AA,H2AB), C3AA(H3AA,H3AB), C4AA(H4AA,H4AB)
4.d Aromatic/amide H refined with riding coordinates:
 C23(H23), C10(H10), C21(H21), C29(H29), C27(H27), C11(H11), C16(H16),
 C12(H12), C15(H15), C14(H14)
4.e Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C34(H34A,H34B,
 H34C), C32(H32A,H32B,H32C), C5(H5A,H5B,H5C), C35(H35A,H35B,H35C), C6(H6A,H6B,
 H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C0AA(H0AA,H0AB,H0AC), C5AA(H5AA,H5AB,
 H5AC)
;
_shelx_res_checksum              42799
_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 1.567
_oxdiff_exptl_absorpt_empirical_full_min 0.602