Snapshots of a solid-state transformation: coexistence of three phases trapped in one crystal
Aromí, G.; Beavers, C. M.; Sánchez Costa, J.; Craig, G. A.; Mínguez Espallargas, G.; Orera, A.; Roubeau, O.; Chem. Sci. 7 (2016) 2907–; doi:10.1039/C5SC04287A

data_1541903
_publ_section_title
;
 Snapshots of a solid-state transformation: coexistence of three phases
 trapped in one crystal
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2907
_journal_paper_doi               10.1039/C5SC04287A
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C36 H30 Fe N10 O2, 2(Cl O4), C3 H6 O'
_chemical_formula_sum            'C39 H36 Cl2 Fe N10 O11'
_chemical_formula_weight         947.53
_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-2013
_audit_update_record
;
2015-03-10 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                71.402(8)
_cell_angle_beta                 68.242(8)
_cell_angle_gamma                67.214(8)
_cell_formula_units_Z            2
_cell_length_a                   12.906(9)
_cell_length_b                   13.199(9)
_cell_length_c                   14.759(10)
_cell_measurement_reflns_used    3947
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.73
_cell_measurement_theta_min      3.08
_cell_volume                     2107(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\p and \w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15425
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        24.900
_diffrn_reflns_theta_max         25.087
_diffrn_reflns_theta_min         2.889
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Bruker AXS Madison WI US'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         5640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1684P)^2^+0.9250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2314
_refine_ls_wR_factor_ref         0.2632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3580
_reflns_number_total             5640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc04287a2.cif
_cod_data_source_block           srj31_Final_LS
_cod_depositor_comments
'Adding full bibliography for 1541896--1541904.cif.'
_cod_database_code               1541903
_shelx_estimated_absorpt_t_min   0.884
_shelx_estimated_absorpt_t_max   0.946
_shelxl_version_number           2013-4
_shelx_res_checksum              17552