Silver(I) complexes with substituted derivatives of the boron cluster anions as ligands
Kubasov, A.S.; Matveev, E. Yu.; Klyukin, I.N.; Nichugovskiy, A.I.; Zhizhin, K. Yu; Kuznetsov, N.T.; Inorganica Chimica Acta 510 (2020) 119749–; doi:10.1016/j.ica.2020.119749

data_1564299
_publ_section_title
;
 Silver(I) complexes with substituted derivatives of the boron cluster
 anions as ligands
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119749
_journal_paper_doi               10.1016/j.ica.2020.119749
_journal_volume                  510
_journal_year                    2020
_chemical_formula_moiety         'C72 H60 Ag P4, C4 H17 B10 O2'
_chemical_formula_sum            'C76 H77 Ag B10 O2 P4'
_chemical_formula_weight         1362.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                73.890(10)
_cell_angle_beta                 84.190(10)
_cell_angle_gamma                89.930(10)
_cell_formula_units_Z            2
_cell_length_a                   14.329(2)
_cell_length_b                   14.682(2)
_cell_length_c                   19.386(3)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    293
_cell_measurement_theta_max      32.230
_cell_measurement_theta_min      27.954
_cell_volume                     3896.6(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17808
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.494
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       block
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.0132(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         15291
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0708
_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^)+(0.1121P)^2^+2.9970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.2253
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9681
_reflns_number_total             15291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2.cif
_cod_data_source_block           b87
_cod_database_code               1564299
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.838
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
2. Restrained distances
 O1-C73 = O1-C76
 1.48 with sigma of 0.01
 C73-C74 = C75-C76
 1.49 with sigma of 0.01
 O2-C74 = O2-C75
 1.42 with sigma of 0.01
 C74-C73
 1.52 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Ag1 \\sim P2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Ag1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(P2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(P1) = Uanis(P2)
Uanis(P3) = Uanis(P2)
Uanis(P4) = Uanis(P2)
4.a Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
4.c Boron cage BH refined with riding coordinates:
 B1(H1), B3(H3A), B4(H4A), B5(H5A), B6(H6A), B7(H7), B8(H8A), B9(H9A), B10(H10A)
;
_shelx_res_checksum              67988
_shelx_hkl_checksum              63107
_shelx_fab_checksum              87942
_olex2_submission_special_instructions 'No special instructions were received'