Control of crystal structure using temperature and time
Zacharias, Savannah C.; Ramon, Gaëlle; Bourne, Susan A.; Acta Crystallographica Section B 74 (2018) –; doi:10.1107/S2052520618007795

data_2108258
_publ_section_title
;
 Control of crystal structure using temperature and time
;
_journal_coeditor_code           LO5021SUP1
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_paper_doi               10.1107/S2052520618007795
_journal_volume                  74
_journal_year                    2018
_chemical_formula_sum            'C48 H40 Fe4 N4 O24'
_chemical_formula_weight         1280.24
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2415(13)
_cell_length_b                   13.2415(13)
_cell_length_c                   14.9977(17)
_cell_measurement_reflns_used    5813
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.865
_cell_measurement_theta_min      2.716
_cell_volume                     2629.7(5)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36874
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.337
_diffrn_reflns_theta_min         2.052
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;G. M. Sheldrick, SADABS, Version 2.05, Univeristy of Gottingen, 
Germany, 2007
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       prism
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.496
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.124
_pd_instr_dist_spec/detc         48
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 1179 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+0.6617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0670
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2913
_reflns_number_total             3279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lo5021sup1.cif
_cod_data_source_block           II
_cod_depositor_comments
;

2019-10-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2629.7(6)
_cod_original_formula_sum        'C12 H10 Fe N O6'
_cod_original_formula_units_Z    8
_cod_original_formula_weight     320.06
_cod_database_code               2108258
_cod_database_fobs_code          2108258
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              77584
_shelx_hkl_checksum              10499