Molecular Squares, Coordination Polymers and Mononuclear Complexes Supported by 2,4-Dipyrazolyl-6H-1,3,5-triazine and 4,6-Dipyrazolylpyrimidine Ligands
Capel Berdiell, Izar; Farmiloe, Sarah E.; Kulmaczewski, Rafal; Halcrow, Malcolm; Dalton Transactions  (2019) –; doi:10.1039/C9DT04003J

data_7701816
_publ_section_title
;
 Molecular Squares, Coordination Polymers and Mononuclear Complexes
 Supported by 2,4-Dipyrazolyl-6H-1,3,5-triazine and
 4,6-Dipyrazolylpyrimidine Ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT04003J
_journal_year                    2019
_chemical_formula_moiety         'C52 H60 Ag4 N28, 4(F6 Sb), C H3 N O2'
_chemical_formula_sum            'C53 H63 Ag4 F24 N29 O2 Sb4'
_chemical_formula_weight         2512.80
_chemical_name_systematic
'Tetrakis-[2,4-di(3,5-dimethylpyrazol-1-yl)-6H-1,3,5-triazine)]-tetrasilver(I) tetra-hexafluoroantimonate nitromethane solvate'
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-08-11
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.028(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.9855(3)
_cell_length_b                   14.9629(3)
_cell_length_c                   23.3614(3)
_cell_measurement_reflns_used    17247
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.73
_cell_measurement_theta_min      3.49
_cell_volume                     8003.8(2)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33503
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.83
_diffrn_reflns_theta_min         3.51
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.250
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4832
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: nitromethane/diethyl ether'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.703
_refine_diff_density_min         -1.703
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1062
_refine_ls_number_reflns         15778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+14.3568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1201
_reflns_number_gt                13737
_reflns_number_total             15778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt04003j2.cif
_cod_data_source_block           sf-23
_cod_database_code               7701816
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C14(H14), C21(H21), C28(H28), C34(H34), C41(H41), C48(H48), C54(H54),
 C61(H61), C68(H68), C74(H74), C81(H81)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C63(H63A,H63B,H63C),
 C64(H64A,H64B,H64C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C83(H83A,H83B,
 H83C), C84(H84A,H84B,H84C), C113(H11A,H11B,H11C)
;