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_7701812
_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(Cl O4), 3.2(C H3 N O2), 1.2(H2 O)'
_chemical_formula_sum            'C55.2 H72 Ag4 Cl4 N31.2 O23.6'
_chemical_formula_weight         2123.52
_chemical_name_systematic
'Tetrakis-[2,4-di(3,5-dimethylpyrazol-1-yl)-1,3,5-triazine]-tetrasilver(I) tetraperchlorate hydrate nitromethane solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-07-08
_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                 107.315(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.8911(9)
_cell_length_b                   27.7398(10)
_cell_length_c                   15.8143(7)
_cell_measurement_reflns_used    8937
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      3.21
_cell_volume                     8749.3(7)
_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 0.997
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'SuperNova, Dual, Mo at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31510
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.54
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.591
_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    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4266
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: nitromethane/diethyl ether'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.372
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         10539
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0742
_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^)+(0.0978P)^2^+86.2927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.2109
_reflns_number_gt                6979
_reflns_number_total             10539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt04003j2.cif
_cod_data_source_block           sf-16
_cod_original_cell_volume        8749.3(6)
_cod_original_formula_sum        'C55.20 H72 Ag4 Cl4 N31.20 O23.60'
_cod_database_code               7701812
_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. Restrained distances
 C54A-N55A = C58A-N59A = C58B-N59B
 1.45 with sigma of 0.02
 N55A-O56A = N55A-O57A = N59A-O60A = N59A-O61A = N59B-O60B = N59B-O61B
 1.22 with sigma of 0.02
 O56A-O57A = O60A-O61A = O60B-O61B
 2.09 with sigma of 0.02
 C54A-O56A = C54A-O57A = C58A-O60A = C58A-O61A = C58B-O60B = C58B-O61B
 2.3 with sigma of 0.02
 C62A-N63A = C62B-N63B = C62C-N63C
 1.45 with sigma of 0.02
 N63A-O64A = N63A-O65A = N63B-O64B = N63B-O65B = N63C-O64C = N63C-O65C
 1.22 with sigma of 0.02
 O64A-O65A = O64B-O65B = O64C-O65C
 2.09 with sigma of 0.02
 C62A-O64A = C62A-O65A = C62B-O64B = C62B-O65B = C62C-O64C = C62C-O65C
 2.3 with sigma of 0.02
 O53-O65B_$1
 -2.8 with sigma of 0.02
3. Others
 Fixed Sof: C54A(0.4) H54A(0.4) H54B(0.4) H54C(0.4) N55A(0.4) O56A(0.4)
 O57A(0.4) O57B(0.6) C58A(0.25) H58A(0.25) H58B(0.25) H58C(0.25) N59A(0.25)
 O60A(0.25) O61A(0.25) C58B(0.25) H58D(0.25) H58E(0.25) H58F(0.25) N59B(0.25)
 O60B(0.25) O61B(0.25) C62A(0.25) H62A(0.25) H62B(0.25) H62C(0.25) N63A(0.25)
 O64A(0.25) O65A(0.25) C62B(0.25) H62D(0.25) H62E(0.25) H62F(0.25) N63B(0.25)
 O64B(0.25) O65B(0.25) C62C(0.2) H62G(0.2) H62H(0.2) H62I(0.2) N63C(0.2)
 O64C(0.2) O65C(0.2)
4.a Me refined with riding coordinates:
 C54A(H54A,H54B,H54C), C58A(H58A,H58B,H58C), C58B(H58D,H58E,H58F), C62A(H62A,
 H62B,H62C), C62B(H62D,H62E,H62F), C62C(H62G,H62H,H62I)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C12(H12), C19(H19), C24(H24), C32(H32), C39(H39)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C)
;