A new family of clusters containing a silver-centered tetracapped [Ag@Ag <sub>4</sub> (μ <sub>3</sub> -P) <sub>4</sub> ] tetrahedron, inscribed within a N <sub>12</sub> icosahedron
Artem'ev, Alexander V.; Bagryanskaya, Irina Yu.; Doronina, Evgeniya P.; Tolstoy, Peter M.; Gushchin, Artem L.; Rakhmanova, Mariana I.; Ivanov, Alexander Yu.; Suturina, Anastasiya O.; Dalton Transactions 46 (2017) 12425–12429; doi:10.1039/C7DT02597A

data_1546806
_publ_section_title
;
 A new family of clusters containing a silver-centered tetracapped [Ag@Ag
 <sub>4</sub> (\m <sub>3</sub> -P) <sub>4</sub> ] tetrahedron, inscribed
 within a N <sub>12</sub> icosahedron
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              12425
_journal_page_last               12429
_journal_paper_doi               10.1039/C7DT02597A
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety
; 
 C69 H63 Ag5 N15 O P4, 5(B F4), C3 H6 O
;
_chemical_formula_sum            'C72 H69 Ag5 B5 F20 N15 O2 P4'
_chemical_formula_weight         2243.15
_chemical_melting_point          503
_chemical_name_systematic
;
 Complex of AgBF4 with tris(2-pyridyl)phosphine
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-08-16 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.970(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.685(3)
_cell_length_b                   22.865(2)
_cell_length_c                   30.599(3)
_cell_measurement_reflns_used    9446
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.37
_cell_volume                     16569(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            245173
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.557
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.337
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.8066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             8836
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.393
_refine_diff_density_min         -1.537
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2185
_refine_ls_number_reflns         37987
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+35.8610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29640
_reflns_number_total             37987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02597a2.cif
_cod_data_source_block           comp2_b6
_cod_depositor_comments
;

2019-02-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        16568(3)
_cod_original_formula_moiety
; 
 C69 H63 Ag5 N15 O P4, C67 H60 Ag5 N14 O P4, C2 N, 10(B F4), C3 H6 O
;
_cod_original_formula_sum        'C141 H129 Ag10 B10 F40 N30 O3 P8'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     4486.29
_cod_database_code               1546806
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.690
_shelx_estimated_absorpt_t_max   0.776
_shelx_res_checksum              80732