Novel hydrogen bond network topologies in complexes of the ditopic ligand 5-amino-3-(pyrid-2-yl)-1H-pyrazole
Jones, Leigh F.; Camm, Kenneth D.; Kilner, Colin A.; Halcrow, Malcolm A.; CrystEngComm 8 (2006) 719–; doi:10.1039/b609424d

data_7203558
_publ_section_title
;
 Novel hydrogen bond network topologies in complexes of the ditopic
 ligand 5-amino-3-(pyrid-2-yl)-1H-pyrazole
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              719
_journal_paper_doi               10.1039/b609424d
_journal_volume                  8
_journal_year                    2006
_chemical_formula_moiety         'C16 H16 Cl2 Fe N8, Cl, 4[C H4 O]'
_chemical_formula_sum            'C20 H32 Cl3 Fe N8 O4'
_chemical_formula_weight         610.74
_chemical_name_systematic
;
Dichloro-bis[5-amino-3-(pyrid-2-yl)pyrazole]iron(III) chloride
tetrakis-methanol solvate (2.4CH~3~OH)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.9291(6)
_cell_angle_beta                 96.0695(6)
_cell_angle_gamma                110.0749(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7275(2)
_cell_length_b                   11.6620(2)
_cell_length_c                   11.9305(2)
_cell_measurement_reflns_used    31506
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.36
_cell_volume                     1378.36(4)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31506
_diffrn_reflns_theta_full        27.30
_diffrn_reflns_theta_max         27.30
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             634
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6159
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0487P)^2^+0.3402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                4977
_reflns_number_total             6159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b609424d.txt
_cod_data_source_block           c:\datasets\leeds\lfj1a\lfj1a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_cell_volume        1378.35(4)
_cod_database_code               7203558