Role of Symmetry Breaking in the Structural Trapping of Light-Induced Excited Spin States
Kulmaczewski, Rafal; Trzop, Elzbieta; Kershaw Cook, Laurence J.; Collet, Eric; CHASTANET, Guillaume; Halcrow, Malcolm; Chemical Communications  (2017) –; doi:10.1039/C7CC07990G

data_7120911
_publ_section_title
;
 Role of Symmetry Breaking in the Structural Trapping of Light-Induced
 Excited Spin States
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C7CC07990G
_journal_year                    2017
_chemical_formula_moiety         'C28 H30 Fe N10 S2, 2(B F4), C H3 N O2'
_chemical_formula_sum            'C29 H33 B2 F8 Fe N11 O2 S2'
_chemical_formula_weight         861.25
_chemical_melting_point          ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2017-07-28 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.942(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7391(7)
_cell_length_b                   11.9252(4)
_cell_length_c                   16.0160(5)
_cell_measurement_reflns_used    2416
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.3170
_cell_measurement_theta_min      3.0060
_cell_volume                     3701.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.37.31c (Rigaku OD, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury3.9 (2016)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1852
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -4.00  97.00   1.00   10.00    --   23.49  38.00-120.00  101
  2  \w    -21.00  22.00   1.00   10.00    --  -21.46 -99.00-150.00   43
  3  \w    -83.00 -34.00   1.00   10.00    --  -21.46 -19.00-120.00   49
  4  \w   -104.00 -45.00   1.00   10.00    --  -21.46 178.00  30.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0006578000
_diffrn_orient_matrix_UB_12      -0.0594618000
_diffrn_orient_matrix_UB_13      -0.0007965000
_diffrn_orient_matrix_UB_21      0.0051500000
_diffrn_orient_matrix_UB_22      -0.0013067000
_diffrn_orient_matrix_UB_23      0.0364809000
_diffrn_orient_matrix_UB_31      -0.0448031000
_diffrn_orient_matrix_UB_32      -0.0010378000
_diffrn_orient_matrix_UB_33      -0.0028020000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.1385
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16453
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         2.975
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         8083
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1363
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0076P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4550
_reflns_number_total             8083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07990g1.cif
_cod_data_source_block           rk137MeNO2_100K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7120911
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32