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_7701824
_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         'C12 H9 Fe N9 S2'
_chemical_formula_sum            'C12 H9 Fe N9 S2'
_chemical_formula_weight         399.25
_chemical_name_systematic
'Catena-[2-amino-4,6-(pyrazol-1-yl)pyrimidine]-di-isothiocyanato iron(II)'
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-07-05
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   16.0404(2)
_cell_length_b                   16.0404(2)
_cell_length_c                   25.1086(3)
_cell_measurement_reflns_used    2639
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.86
_cell_measurement_theta_min      1.46
_cell_volume                     6460.30(14)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.855
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13505
_diffrn_reflns_theta_full        24.82
_diffrn_reflns_theta_max         24.91
_diffrn_reflns_theta_min         1.46
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.114
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Sheldrick, 2002).  University of Gottingen, Germany.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3232
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         2629
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0558
_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^)+(0.1050P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1753
_reflns_number_gt                1383
_reflns_number_total             2629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt04003j2.cif
_cod_data_source_block           90-ncs
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7701824
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H,H) groups
2. Restrained distances
 N14-H14A = N14-H14B
 0.9 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24)
;
_olex2_submission_special_instructions 'No special instructions were received'