Direct synthesis of an anionic 13-vertex closo-cobaltacarborane cluster.
Maier, Thomas M.; Coburger, Peter; van Leest, Nicolaas P.; Hey-Hawkins, Evamarie; Wolf, Robert; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15772–15777; doi:10.1039/c9dt03111a

data_7701306
_publ_section_title
;
 Direct synthesis of an anionic 13-vertex closo-cobaltacarborane cluster.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15772
_journal_page_last               15777
_journal_paper_doi               10.1039/c9dt03111a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C56 H58 B10 Co N2 P2'
_chemical_formula_sum            'C56 H58 B10 Co N2 P2'
_chemical_formula_weight         988.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-04
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2019-07-29 deposited with the CCDC.    2019-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.950(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2578(2)
_cell_length_b                   24.1038(4)
_cell_length_c                   19.6169(3)
_cell_measurement_reflns_used    8545
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.7850
_cell_measurement_theta_min      3.9150
_cell_volume                     5284.04(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_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 0.989
_diffrn_measured_fraction_theta_max 0.962
_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      4.00  94.00   1.00    3.00    --   42.41-125.00-120.00   90
  2  \w    -30.00  63.00   1.00    3.00    --   42.41 -37.00 -60.00   93
  3  \w     30.00  69.00   1.00    8.00    --  106.40 -30.00-180.00   39
  4  \w     28.00  96.00   1.00    8.00    --  106.40 -94.00 -90.00   68
  5  \w     74.00 148.00   1.00    8.00    --  106.40 125.00-120.00   74
  6  \w     61.00 154.00   1.00    8.00    --  106.40  15.00-150.00   93
  7  \w     33.00  69.00   1.00    8.00    --  106.40 -30.00 -60.00   36
  8  \w    100.00 158.00   1.00    8.00    --  106.40 125.00  90.00   58
  9  \w     74.00 158.00   1.00    8.00    --  106.40 125.00-150.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0530449000
_diffrn_orient_matrix_UB_12      0.0253136000
_diffrn_orient_matrix_UB_13      0.0691471000
_diffrn_orient_matrix_UB_21      -0.0698719000
_diffrn_orient_matrix_UB_22      -0.0424313000
_diffrn_orient_matrix_UB_23      0.0382447000
_diffrn_orient_matrix_UB_31      0.1064019000
_diffrn_orient_matrix_UB_32      -0.0405630000
_diffrn_orient_matrix_UB_33      0.0031430000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20536
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.844
_diffrn_reflns_theta_min         3.668
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.406
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.18b (Rigaku Oxford Diffraction, 2018)
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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.176
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         10282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+2.9082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9233
_reflns_number_total             10282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03111a2.cif
_cod_data_source_block           mp_abs
_cod_depositor_comments
'Adding full bibliography for 7701305--7701307.cif.'
_cod_database_code               7701306
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C224  H232  B40  Co4  N8  P8  '
_chemical_oxdiff_usercomment     'Hexanmutterlauge nach mehreren Tagen'
_reflns_odcompleteness_completeness 99.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C15(H15), C17(H17),
 C24(H24), C26(H26), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40),
  C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48),
 C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
2.c Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4A), B5(H5A), B6(H6A), B7(H7), B8(H8A), B9(H9A),
 B10(H10A)
;
_shelx_res_checksum              38450
_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 1.923
_oxdiff_exptl_absorpt_empirical_full_min 0.634