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_2108257
_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_page_first
;
;
_journal_paper_doi               10.1107/S2052520618007795
_journal_volume                  74
_journal_year                    2018
_chemical_formula_moiety         'C14 H15 Fe N2 O7'
_chemical_formula_sum            'C14 H15 Fe N2 O7'
_chemical_formula_weight         379.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                93.169(5)
_cell_angle_beta                 100.097(4)
_cell_angle_gamma                99.996(4)
_cell_formula_units_Z            2
_cell_length_a                   8.6448(17)
_cell_length_b                   9.0260(18)
_cell_length_c                   10.773(2)
_cell_measurement_reflns_used    22935
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.515
_cell_measurement_theta_min      1.928
_cell_volume                     811.8(3)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_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  0.0402
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22935
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.515
_diffrn_reflns_theta_min         1.928
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; G. M. Sheldrick, SADABS, Version 2.05, University of Gottingen, 
Germany, 2007
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       block
_exptl_crystal_F_000             390
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0066(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         4072
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0312P)^2^+0.3567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3573
_reflns_number_total             4072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lo5021sup1.cif
_cod_data_source_block           I
_cod_database_code               2108257
_cod_database_fobs_code          2108257
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.815
_shelx_estimated_absorpt_t_max   0.838
_shelx_res_checksum              76205
_shelx_hkl_checksum              79873