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_7701307
_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         'C38 H40 Co N2, C3 H7'
_chemical_formula_sum            'C41 H47 Co N2'
_chemical_formula_weight         626.73
_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             2019-01-22
_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                102.644(6)
_cell_angle_beta                 95.457(7)
_cell_angle_gamma                97.860(8)
_cell_formula_units_Z            2
_cell_length_a                   8.1878(9)
_cell_length_b                   10.6068(9)
_cell_length_c                   19.8411(13)
_cell_measurement_reflns_used    3362
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      74.0840
_cell_measurement_theta_min      4.2840
_cell_volume                     1651.6(3)
_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 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.976
_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    -68.00  28.00   1.00    8.00    --  -42.56  57.00 120.00   96
  2  \w   -113.00 -16.00   1.00    8.00    --  -42.56 -57.00 -30.00   97
  3  \w    -20.00  76.00   1.00    8.00    --   42.56 -99.00-120.00   96
  4  \w     38.00 133.00   1.00   32.00    --  106.63 -77.00-120.00   95
  5  \w     26.00 101.00   1.00   32.00    --  106.63 -94.00 120.00   75
  6  \w     31.00 104.00   1.00   32.00    --  106.63 -94.00  60.00   73
  7  \w     35.00  77.00   1.00   32.00    --  106.63 -45.00  90.00   42
  8  \w     35.00  63.00   1.00   32.00    --  106.63 -30.00-180.00   28
  9  \w     32.00  68.00   1.00   32.00    --  106.63 -30.00 120.00   36
 10  \w     34.00  66.00   1.00   32.00    --  106.63 -30.00 150.00   32
 11  \w     56.00 122.00   1.00   32.00    --  106.63-125.00-120.00   66
 12  \w     84.00 154.00   1.00   32.00    --  106.63  45.00  90.00   70
 13  \w     49.00 115.00   1.00   32.00    --  106.63-125.00  60.00   66
 14  \w     63.00 149.00   1.00   32.00    --  106.63  15.00  60.00   86
 15  \w     61.00 158.00   1.00   32.00    --  106.63  15.00 -30.00   97
 16  \w     32.00  57.00   1.00   32.00    --  106.63 -30.00 -90.00   25
;
_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      -0.0600698000
_diffrn_orient_matrix_UB_12      0.0936345000
_diffrn_orient_matrix_UB_13      -0.0428132000
_diffrn_orient_matrix_UB_21      -0.1767720000
_diffrn_orient_matrix_UB_22      -0.0306672000
_diffrn_orient_matrix_UB_23      0.0190776000
_diffrn_orient_matrix_UB_31      0.0428184000
_diffrn_orient_matrix_UB_32      0.1142291000
_diffrn_orient_matrix_UB_33      0.0651382000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9999
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.081
_diffrn_reflns_theta_min         4.329
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.294
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.312
_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            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       prism
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.423
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.985
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0683
_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^)+(0.0559P)^2^+2.7211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5418
_reflns_number_total             6275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03111a2.cif
_cod_data_source_block           ap
_cod_depositor_comments
'Adding full bibliography for 7701305--7701307.cif.'
_cod_original_cell_volume        1651.5(3)
_cod_database_code               7701307
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C82 Co2 N4 H1 '
_chemical_oxdiff_usercomment     'Hexan aus Reaktion mit Carboran'
_reflns_odcompleteness_completeness 97.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H00A(0.04) H00B(0.04) H00C(0.04) H4(0.03) H5(0.034) H6(0.034)
 H8(0.034) H9(0.034) H10(0.027) H15(0.029) H17(0.028) H19A(0.042) H19B(0.042)
 H19C(0.042) H20A(0.048) H20B(0.048) H20C(0.048) H21A(0.04) H21B(0.04)
 H21C(0.04) H24(0.026) H26(0.027) H28A(0.037) H28B(0.037) H28C(0.037)
 H29A(0.044) H29B(0.044) H29C(0.044) H31(0.027) H32(0.028) H33A(0.037)
 H33B(0.037) H34A(0.03) H34B(0.03) H35(0.025) H36(0.025) H37A(0.032)
 H37B(0.032) H38A(0.029) H38B(0.029) H39A(0.078) H39B(0.078) H39C(0.078)
 H40A(0.055) H40B(0.055) H41A(0.044) H41B(0.044)
 Fixed X: H00A(1.081625) H00B(1.2435) H00C(1.101911) H4(0.438852) H5(0.40502)
 H6(0.522306) H8(0.703125) H9(0.845736) H10(0.864952) H15(0.14782)
 H17(0.589017) H19A(0.288442) H19B(0.1285) H19C(0.256021) H20A(0.206858)
 H20B(0.186015) H20C(0.347951) H21A(0.828444) H21B(0.843402) H21C(0.842711)
 H24(0.821892) H26(1.2419) H28A(0.545444) H28B(0.562558) H28C(0.558753)
 H29A(1.089466) H29B(1.257536) H29C(1.154836) H31(0.678997) H32(0.446486)
 H33A(0.462935) H33B(0.395496) H34A(0.590578) H34B(0.707319) H35(0.743761)
 H36(0.972691) H37A(1.002208) H37B(1.045062) H38A(0.872019) H38B(0.767136)
 H39A(1.038027) H39B(1.17266) H39C(0.985385) H40A(1.089374) H40B(0.897971)
 H41A(1.122517) H41B(0.926683)
 Fixed Y: H00A(0.393436) H00B(0.4913) H00C(0.436529) H4(0.064749) H5(0.093183)
 H6(0.281729) H8(0.519262) H9(0.674806) H10(0.641699) H15(-0.106382) H17(-
 0.233388) H19A(0.210411) H19B(0.116508) H19C(0.201039) H20A(-0.342041) H20B(-
 0.351143) H20C(-0.390271) H21A(0.02229) H21B(-0.087227) H21C(0.061173)
 H24(0.870628) H26(0.720913) H28A(0.624022) H28B(0.736682) H28C(0.587434)
 H29A(1.00788) H29B(0.949678) H29C(0.989904) H31(0.053045) H32(0.135201)
 H33A(0.213325) H33B(0.310162) H34A(0.454222) H34B(0.346753) H35(0.520738)
 H36(0.442858) H37A(0.308089) H37B(0.243293) H38A(0.072917) H38B(0.164598)
 H39A(0.381904) H39B(0.304387) H39C(0.280779) H40A(0.204617) H40B(0.19359)
 H41A(0.053928) H41B(0.036377)
 Fixed Z: H00A(0.321813) H00B(0.315554) H00C(0.250246) H4(0.095928) H5(-
 0.018831) H6(-0.047449) H8(-0.001754) H9(0.092338) H10(0.206147) H15(0.19604)
 H17(0.187072) H19A(0.285761) H19B(0.239625) H19C(0.203859) H20A(0.1146)
 H20B(0.192861) H20C(0.159662) H21A(0.183031) H21B(0.226395) H21C(0.266234)
 H24(0.373784) H26(0.340844) H28A(0.292903) H28B(0.362766) H28C(0.367103)
 H29A(0.352294) H29B(0.363781) H29C(0.427689) H31(0.36084) H32(0.367281)
 H33A(0.497348) H33B(0.453632) H34A(0.530466) H34B(0.537067) H35(0.450701)
 H36(0.424072) H37A(0.512721) H37B(0.437054) H38A(0.453707) H38B(0.501762)
 H39A(0.073412) H39B(0.102582) H39C(0.119725) H40A(-0.013889) H40B(-0.002122)
 H41A(0.058975) H41B(0.062229)
;
_shelx_res_checksum              31307
_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 1.990
_oxdiff_exptl_absorpt_empirical_full_min 0.546