Formation of a Cationic Calcium Hydride Cluster with a "Naked" Triphenylsilyl Anion by Hydrogenolysis of Bis(triphenylsilyl)calcium.
Leich, Valeri; Spaniol, Thomas P.; Okuda, Jun; Inorganic chemistry 54 (2015) 4927–4933; doi:10.1021/acs.inorgchem.5b00527

data_4342888
_publ_section_title
;
 Formation of a Cationic Calcium Hydride Cluster with a &quot;Naked&quot;
 Triphenylsilyl Anion by Hydrogenolysis of Bis(triphenylsilyl)calcium.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4927
_journal_page_last               4933
_journal_paper_doi               10.1021/acs.inorgchem.5b00527
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C33 H77 Ca3 N12, C18 H15 Si, 2(C4 H8 O)'
_chemical_formula_sum            'C59 H108 Ca3 N12 O2 Si'
_chemical_formula_weight         1165.90
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.2498(18)
_cell_length_b                   14.2498(18)
_cell_length_c                   18.506(3)
_cell_measurement_reflns_used    2230
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.56
_cell_measurement_theta_min      2.75
_cell_volume                     3254.3(8)
_computing_cell_refinement       'Bruker SMART (2001)'
_computing_data_collection       'Bruker SMART (2001)'
_computing_data_reduction        'Bruker SAINT+ (1999)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1139
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38306
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.427
_diffrn_reflns_theta_min         1.650
_exptl_absorpt_coefficient_mu    0.321
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs Bruker'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 1691 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4459
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0428P)^2^+2.6075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1314
_reflns_Friedel_coverage         0.992
_reflns_friedel_fraction_full    0.999
_reflns_friedel_fraction_max     0.996
_reflns_number_gt                3830
_reflns_number_total             4459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00527_si_002.cif
_cod_data_source_block           4a
_cod_depositor_comments          'Adding full bibliography for 4342888.cif.'
_cod_original_cell_volume        3254.3(10)
_cod_database_code               4342888
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.962
_shelxl_version_number           2013-4
_shelx_res_checksum              87235
_shelx_hkl_checksum              90512