From alkaline earth to coinage metal carboranyls.
Pearce, Kyle G.; Morris, Louis J.; Robinson, Thomas P.; Johnson, Andrew L.; Mahon, Mary F.; Hill, Michael S.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6653–6659; doi:10.1039/d4dt00478g

data_7715484
_publ_section_title
;
 From alkaline earth to coinage metal carboranyls.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6653
_journal_page_last               6659
_journal_paper_doi               10.1039/d4dt00478g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C31 H52 B10 Ca N2'
_chemical_formula_sum            'C31 H52 B10 Ca N2'
_chemical_formula_weight         600.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-14 deposited with the CCDC.	2024-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5052(8)
_cell_length_b                   11.9353(3)
_cell_length_c                   13.8858(5)
_cell_measurement_reflns_used    5094
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      69.7980
_cell_measurement_theta_min      4.1120
_cell_volume                     3564.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0950
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21906
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.477
_diffrn_reflns_theta_min         3.703
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.670
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.492(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         5999
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0844P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1620
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                4936
_reflns_number_total             5999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00478g2.cif
_cod_data_source_block           s23msh104-cpd-2
_cod_depositor_comments
'Adding full bibliography for 7715481--7715486.cif.'
_cod_database_code               7715484
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.864
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.508(17)
 0.492(17)
2. 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
3. Restrained distances
 B6-H6 = B10-H10A = B7-H7
 1.12 with sigma of 0.005
4.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
4.d Boron cage BH refined with riding coordinates:
 C31(H31), B1(H1), B2(H2), B3(H3A), B4(H4), B5(H5), B8(H8A), B9(H9A)
;
_shelx_res_checksum              5984
_olex2_submission_special_instructions 'No special instructions were received'