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_7701822
_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         'C10 H11 Fe N6 O2, 2(Cl O4)'
_chemical_formula_sum            'C10 H12 Cl2 Fe N6 O10'
_chemical_formula_weight         503.01
_chemical_name_systematic
;
Catena-[4,6-(pyrazol-1-yl)pyrimidine]-diaquairon(II) diperchlorate
;
_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             2019-07-05
_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                 113.519(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.888(2)
_cell_length_b                   9.323(2)
_cell_length_c                   19.916(2)
_cell_measurement_reflns_used    1585
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      73.34
_cell_measurement_theta_min      5.17
_cell_volume                     3556.2(10)
_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      125(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.965
_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  0.0387
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6362
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.24
_diffrn_reflns_theta_min         4.62
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.228
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.557
_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            yellow
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2032
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: nitromethane'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3454
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0881
_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^)+(0.1130P)^2^+27.6726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2258
_refine_ls_wR_factor_ref         0.2503
_reflns_number_gt                2515
_reflns_number_total             3454
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt04003j2.cif
_cod_data_source_block           icb15nm
_cod_original_cell_volume        3556.3(10)
_cod_database_code               7701822
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 Cl1A-O22A = Cl1A-O23A = Cl1A-O24A = Cl1A-O25A
 1.4318 with sigma of 0.02
 Cl1B-O22B = Cl1B-O23B = Cl1B-O24B = Cl1B-O25B
 1.4318 with sigma of 0.02
 O22A-O23A = O22A-O24A = O22A-O25A = O23A-O24A = O23A-O25A = O24A-O25A
 2.338129 with sigma of 0.02
 O22B-O23B = O22B-O24B = O22B-O25B = O23B-O24B = O23B-O25B = O24B-O25B
 2.338129 with sigma of 0.02
 Cl6A-O27A = Cl6A-O28A = Cl6A-O29A = Cl6A-O30A
 1.4318 with sigma of 0.02
 Cl6B-O27B = Cl6B-O28B = Cl6B-O29B = Cl6B-O30B
 1.4318 with sigma of 0.02
 O27A-O28A = O27A-O29A = O27A-O30A = O28A-O29A = O28A-O30A = O29A-O30A
 2.338129 with sigma of 0.02
 O27B-O28B = O27B-O29B = O27B-O30B = O28B-O29B = O28B-O30B = O29B-O30B
 2.338129 with sigma of 0.02
 O19-H19A = O19-H19B = O20-H20
 0.9 with sigma of 0.02
 H19A-H19B
 1.37 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: Cl1A(0.5) O22A(0.5) O23A(0.5) O24A(0.5) O25A(0.5) Cl1B(0.5)
 O22B(0.5) O23B(0.5) O24B(0.5) O25B(0.5) Cl6A(0.6) O27A(0.6) O28A(0.6)
 O29A(0.6) O30A(0.6) Cl6B(0.4) O27B(0.4) O28B(0.4) O29B(0.4) O30B(0.4)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C18(H18)
;