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_1546807
_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
;
 C64 H47 Ag5 F12 N12 O12 P4 S4, C F3 O3 S, 6(C3 H6 O)
;
_chemical_formula_sum            'C83 H83 Ag5 F15 N12 O21 P4 S5'
_chemical_formula_weight         2693.14
_chemical_melting_point          546(19)
_chemical_name_systematic
;
 Complex of AgOTf 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                 105.155(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4246(7)
_cell_length_b                   22.9762(11)
_cell_length_c                   28.4848(11)
_cell_measurement_reflns_used    9413
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.93
_cell_measurement_theta_min      2.19
_cell_volume                     10375.6(8)
_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 0.984
_diffrn_measured_fraction_theta_max 0.949
_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  0.0338
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            93670
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.038
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.187
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5372
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.600
_exptl_crystal_size_min          0.400
_refine_diff_density_max         2.220
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1372
_refine_ls_number_reflns         22569
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0058P)^2^+115.6130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17200
_reflns_number_total             22569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02597a2.cif
_cod_data_source_block           comp1_b53
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '527-565' was changed to '546(19)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               1546807
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.536
_shelx_estimated_absorpt_t_max   0.648
_shelx_res_checksum              9905