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_7120902
_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, C2 H3 N, 2(B F4)'
_chemical_formula_sum            'C30 H33 B2 F8 Fe N11 S2'
_chemical_formula_weight         841.26
_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                 99.208(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2280(5)
_cell_length_b                   11.8526(4)
_cell_length_c                   15.5284(4)
_cell_measurement_reflns_used    4950
_cell_measurement_temperature    15(1)
_cell_measurement_theta_max      31.6220
_cell_measurement_theta_min      3.1820
_cell_volume                     3675.03(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.37.31c (Rigaku OD, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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      15(1)
_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 0.998
_diffrn_measurement_details
;
  1 omega   12.00  105.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       32.4262   38.0000   30.0000 93

  2 omega  -57.00   -2.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -30.3949    0.0000 -180.0000 55

  3 omega  -77.00  -37.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -30.3949  103.0000  156.3300 40

  4 omega -109.00  -56.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -30.3949 -178.0000 -180.0000 53

  5 omega  -90.00  -63.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -30.3949 -178.0000 -150.0000 27

  6 omega -109.00  -59.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -30.3949 -178.0000    0.0000 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0008170000
_diffrn_orient_matrix_UB_12      -0.0562197000
_diffrn_orient_matrix_UB_13      0.0118714000
_diffrn_orient_matrix_UB_21      -0.0055698000
_diffrn_orient_matrix_UB_22      0.0203727000
_diffrn_orient_matrix_UB_23      0.0320145000
_diffrn_orient_matrix_UB_31      -0.0459424000
_diffrn_orient_matrix_UB_32      -0.0014941000
_diffrn_orient_matrix_UB_33      -0.0098303000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19748
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         3.081
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            'light orange'
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.5026
_exptl_crystal_size_mid          0.1566
_exptl_crystal_size_min          0.0797
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0530P)^2^+0.7738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1275
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5813
_reflns_number_total             7998
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07990g1.cif
_cod_data_source_block           rk137MeCNPI_015K
_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               7120902
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32