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_1541898
_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),1.25(C3 H6 O)'
_chemical_formula_sum            'C39.75 H37.5 Cl2 Fe N10 O11.25'
_chemical_formula_weight         962.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-22 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.290(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.165(5)
_cell_length_b                   21.596(8)
_cell_length_c                   15.414(6)
_cell_measurement_reflns_used    1221
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      24.6
_cell_measurement_theta_min      2.68
_cell_volume                     4298(3)
_computing_cell_refinement       'SAINT V8.27B(Bruker, 2012)'
_computing_data_collection       'Apex2 v2012.10-0 (Bruker, 2012)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
         SHELXTL 5.1, XP (Sheldrick, 1994)
    ShelXle Rev 699 (Hubschle, 2011)
;
_computing_publication_material  SHELXL-2014/7
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.250
_diffrn_measured_fraction_theta_max 0.261
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_type       'Sparks (1982)'
_diffrn_orient_matrix_UB_11      -0.04852
_diffrn_orient_matrix_UB_12      0.01369
_diffrn_orient_matrix_UB_13      0.02844
_diffrn_orient_matrix_UB_21      0.01050
_diffrn_orient_matrix_UB_22      -0.04028
_diffrn_orient_matrix_UB_23      0.03475
_diffrn_orient_matrix_UB_31      0.05945
_diffrn_orient_matrix_UB_32      0.01829
_diffrn_orient_matrix_UB_33      0.05523
_diffrn_radiation_monochromator  silicon(111)
_diffrn_radiation_source         'Advanced Light Source Beamline 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.250
_diffrn_reflns_Laue_measured_fraction_max 0.261
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4017
_diffrn_reflns_point_group_measured_fraction_full 0.250
_diffrn_reflns_point_group_measured_fraction_max 0.261
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         28.046
_diffrn_reflns_theta_min         2.681
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1  (Sheldrick, 2012)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         2103
_refine_ls_number_restraints     904
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0771
_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^)+(0.1345P)^2^+5.4453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2095
_refine_ls_wR_factor_ref         0.2322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1487
_reflns_number_total             2103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc04287a2.cif
_cod_data_source_block           Stage2_Initial
_cod_depositor_comments
'Adding full bibliography for 1541896--1541904.cif.'
_cod_original_formula_sum        'C39.75 H37.50 Cl2 Fe N10 O11.25'
_cod_database_code               1541898
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.934
_shelx_estimated_absorpt_t_max   0.966
_shelx_res_checksum              93369