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_7701305
_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         'C68 H88 B10 Co K N2 O6 P2'
_chemical_formula_sum            'C68 H88 B10 Co K N2 O6 P2'
_chemical_formula_weight         1297.47
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-03
_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                 95.5970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.96290(10)
_cell_length_b                   13.7270(2)
_cell_length_c                   36.1365(4)
_cell_measurement_reflns_used    15025
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.8580
_cell_measurement_theta_min      4.0240
_cell_volume                     6893.22(14)
_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 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_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    -70.00  25.00   1.00    2.50    --  -44.88  57.00-180.00   95
  2  \w   -122.00 -12.00   1.00    2.50    --  -44.88 -19.00   0.00  110
  3  \w     22.00 109.00   1.00   10.00    --  104.50 -95.00 -32.00   87
  4  \w     80.00 175.00   1.00   10.00    --  104.50  45.00   0.00   95
  5  \w     80.00 175.00   1.00   10.00    --  104.50  45.00 -60.00   95
  6  \w     42.00 117.00   1.00   10.00    --  104.50-125.00  90.00   75
  7  \w     33.00 112.00   1.00   10.00    --  104.50-125.00 -90.00   79
  8  \w    118.00 178.00   1.00   10.00    --  104.50 125.00  30.00   60
;
_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      -0.0259518000
_diffrn_orient_matrix_UB_12      -0.0441547000
_diffrn_orient_matrix_UB_13      0.0369185000
_diffrn_orient_matrix_UB_21      -0.0136934000
_diffrn_orient_matrix_UB_22      0.1031986000
_diffrn_orient_matrix_UB_23      0.0154579000
_diffrn_orient_matrix_UB_31      -0.1068543000
_diffrn_orient_matrix_UB_32      -0.0021766000
_diffrn_orient_matrix_UB_33      -0.0152762000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            32794
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.889
_diffrn_reflns_theta_min         3.446
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.326
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.204
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.526
_exptl_crystal_size_mid          0.294
_exptl_crystal_size_min          0.161
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         13569
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0454P)^2^+2.3354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12219
_reflns_number_total             13569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03111a2.cif
_cod_data_source_block           mp_neu
_cod_depositor_comments
'Adding full bibliography for 7701305--7701307.cif.'
_cod_database_code               7701305
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C272  H328  B40  Co4  K4  N8  O24  P8  '
_reflns_odcompleteness_completeness 99.76
_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, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-C62 \\sim O2-C59A \\sim O2-C63 \\sim O2-C60A
 with sigma of 0.02
 C62-C61 \\sim C59A-C58A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C58A \\sim C59A \\sim C60A \\sim C61 \\sim C62 \\sim C63: within 2A with sigma
of 0.05 and sigma for terminal atoms of 0.05
4. Others
 Sof(C59A)=Sof(H59D)=Sof(H59E)=1-FVAR(1)
 Sof(C62)=Sof(H62A)=Sof(H62B)=FVAR(1)
 Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(2)
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(2)
 Sof(C58A)=Sof(H58C)=Sof(H58D)=1-FVAR(3)
 Sof(C61)=Sof(H61A)=Sof(H61B)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C58(H58A,H58B), C58A(H58C,H58D), C59A(H59D,H59E), C61(H61A,
 H61B), C62(H62A,H62B), C65(H65A,H65B), C66(H66A,H66B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C16(H16), C18(H18),
 C25(H25), C27(H27), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C39(H39),
  C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C47(H47),
 C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
5.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C56(H56A,H56B,H56C), C59(H59A,
 H59B,H59C), C60(H60A,H60B,H60C), C60A(H60D,H60E,H60F), C63(H63A,H63B,H63C),
 C64(H64A,H64B,H64C), C67(H67A,H67B,H67C)
5.d Boron cage BH refined with riding coordinates:
 B1(H1), B3(H3), B4(H4), B5(H5), B6(H6A), B7(H7A), B8(H8A), B9(H9), B10(H10A)
;
_shelx_res_checksum              73246
_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 1.382
_oxdiff_exptl_absorpt_empirical_full_min 0.743