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_7701815
_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         'C68 H76 Ag4 N28, 4(Cl O4), C H3 N O2'
_chemical_formula_sum            'C69 H79 Ag4 Cl4 N29 O18'
_chemical_formula_weight         2175.89
_chemical_name_systematic
'Tetrakis-[2,4-di(4,5,6,7-tetrahydroindazol-2-yl)-6H-1,3,5-triazine]-tetrasilver(I) tetraperchlorate 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             2019-07-09
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2019-11-03 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 131.404(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.7165(11)
_cell_length_b                   33.8226(13)
_cell_length_c                   15.6449(6)
_cell_measurement_reflns_used    3162
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.40
_cell_measurement_theta_min      4.83
_cell_volume                     8222.3(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 0.841
_diffrn_measured_fraction_theta_max 0.824
_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  0.0554
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10874
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.85
_diffrn_reflns_theta_min         4.59
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.462
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.714
_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    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4384
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: nitromethane-diethyl ether'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.288
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         6881
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+43.6977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                4861
_reflns_number_total             6881
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt04003j2.cif
_cod_data_source_block           sf26-3
_cod_original_cell_volume        8222.3(6)
_cod_database_code               7701815
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl5A-O57A = Cl5A-O58A = Cl5A-O59A = Cl5A-O60A
 1.43 with sigma of 0.02
 Cl5B-O57B = Cl5B-O58B = Cl5B-O59B = Cl5B-O60B
 1.43 with sigma of 0.02
 O57A-O58A = O57A-O59A = O57A-O60A = O58A-O59A = O58A-O60A = O59A-O60A
 2.34 with sigma of 0.02
 O57B-O58B = O57B-O59B = O57B-O60B = O58B-O59B = O58B-O60B = O59B-O60B
 2.34 with sigma of 0.02
 C69-N70
 1.45 with sigma of 0.02
 N70-O71 = N70-O72
 1.22 with sigma of 0.02
 O71-O72
 2.09 with sigma of 0.02
 C69-O71 = C69-O72
 2.34 with sigma of 0.02
3. Others
 Fixed Sof: Cl51(0.5) O52(0.5) O53(0.5) O54(0.5) O55(0.5) Cl5A(0.33)
 O57A(0.33) O58A(0.33) O59A(0.33) O60A(0.33) Cl5B(0.17) O57B(0.17) O58B(0.17)
 O59B(0.17) O60B(0.17) Cl61(0.5) O62(0.5) O63(0.5) O64(0.5) O65(0.5) C69(0.5)
 H69A(0.5) H69B(0.5) H69C(0.5) N70(0.5) O71(0.5) O72(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C45(H45A,H45B), C46(H46A,H46B),
  C47(H47A,H47B), C48(H48A,H48B)
4.b Me refined with riding coordinates:
 C69(H69A,H69B,H69C)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C17(H17), C26(H26), C30(H30), C41(H41), C50(H50)
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