Syntheses, Structural Variation, and Characterization of a Series of Crystalline Coordination Compounds with 4-Benzene-1,2,4-triazole: Polymorph, Incomplete Spin Transition, and Single Crystal-to-Single Crystal Transformation
Wu, Xiang Xia; Wang, You You; Yang, Pan; Xu, Yao Yao; Huo, Jian Zhong; Ding, Bin; Wang, Ying; Wang, XiuGuang; Crystal Growth & Design 14 (2014) 477–; doi:10.1021/cg401141a

data_4509922
_publ_section_title
;
 Syntheses, Structural Variation, and Characterization of a Series of
 Crystalline Coordination Compounds with 4-Benzene-1,2,4-triazole:
 Polymorph, Incomplete Spin Transition, and Single Crystal-to-Single
 Crystal Transformation
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              477
_journal_paper_doi               10.1021/cg401141a
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C48 H47 Fe2 N19 O2 S4'
_chemical_formula_weight         1161.96
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6608(3)
_cell_length_b                   17.6843(3)
_cell_length_c                   17.8456(4)
_cell_measurement_reflns_used    6285
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1863
_cell_measurement_theta_min      2.4400
_cell_volume                     5257.93(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14148
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.8612
_exptl_absorpt_correction_T_min  0.8132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.692
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.018(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         8968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0530P)^2^+5.6185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                7770
_reflns_number_total             8968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401141a_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NONE' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        5257.92(17)
_cod_original_sg_symbol_H-M      P212121
_cod_original_formula_sum        'C8.35 H8.17 Fe0.35 N3.30 O0.35 S0.70'
_cod_database_code               4509922