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_7701823
_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         'C17 H19 N7, 2(C H Cl3)'
_chemical_formula_sum            'C19 H21 Cl6 N7'
_chemical_formula_weight         560.13
_chemical_name_systematic
'2,4-Bis(4,5,6,7-tetrahydroindazol-2-yl)-6H-1,3,5-triazinedichloroform solvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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
;
2019-10-04 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                88.648(2)
_cell_angle_beta                 86.046(3)
_cell_angle_gamma                87.961(2)
_cell_formula_units_Z            4
_cell_length_a                   9.3073(3)
_cell_length_b                   11.3030(3)
_cell_length_c                   23.5856(8)
_cell_measurement_reflns_used    6346
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.19
_cell_measurement_theta_min      3.73
_cell_volume                     2473.19(13)
_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 0.945
_diffrn_measured_fraction_theta_max 0.932
_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  0.0524
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19525
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.79
_diffrn_reflns_theta_min         3.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.530
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.421
_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    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1144
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         9320
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.819
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1155P)^2^+3.3688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1950
_refine_ls_wR_factor_ref         0.2201
_reflns_number_gt                6794
_reflns_number_total             9320
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt04003j2.cif
_cod_data_source_block           sf-3
_cod_database_code               7701823
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C57A-Cl8A = C57A-Cl9A = C57A-Cl0A = C57B-Cl8B = C57B-Cl9B = C57B-Cl0B
 1.72 with sigma of 0.02
 Cl8A-Cl9A = Cl8A-Cl0A = Cl9A-Cl0A = Cl8B-Cl9B = Cl8B-Cl0B = Cl9B-Cl0B
 2.81 with sigma of 0.02
 C61A-Cl2A = C61A-Cl3A = C61A-Cl4A = C61B-Cl2B = C61B-Cl3B = C61B-Cl4B
 1.72 with sigma of 0.02
 Cl2A-Cl2A = Cl2A-Cl4A = Cl3A-Cl4A = Cl2B-Cl3B = Cl2B-Cl4B = Cl3B-Cl4B
 2.81 with sigma of 0.02
3. Others
 Fixed Sof: C57A(0.61) H57A(0.61) Cl8A(0.61) Cl9A(0.61) Cl0A(0.61) C57B(0.39)
 H57B(0.39) Cl8B(0.39) Cl9B(0.39) Cl0B(0.39) C61A(0.64) H61A(0.64) Cl2A(0.64)
 Cl3A(0.64) Cl4A(0.64) C61B(0.36) H61B(0.36) Cl2B(0.36) Cl3B(0.36) Cl4B(0.36)
4.a Ternary CH refined with riding coordinates:
 C49(H49), C53(H53), C57A(H57A), C57B(H57B), C61A(H61A), C61B(H61B)
4.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C19(H19A,
 H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C43(H43A,H43B), C44(H44A,H44B),
  C45(H45A,H45B), C46(H46A,H46B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C15(H15), C24(H24), C28(H28), C39(H39), C48(H48)
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