Using polymorphism to master the spin crossover mechanism in [Fe(PM-PeA)2(NCSe)2]
Tailleur, Elodie; Marchivie, Mathieu; Negrier, Philippe; Denux, Dominique; Massip, Stéphane; Mondieig, Denise; Chastanet, Guillaume; Guionneau, Philippe; CrystEngComm 21 (2019) 6246–; doi:10.1039/C9CE01137D

data_7234441
_publ_section_title
;
 Using polymorphism to master the spin crossover mechanism in
 [Fe(PM-PeA)2(NCSe)2]
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              6246
_journal_paper_doi               10.1039/C9CE01137D
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C42 H28 Fe N6 Se2'
_chemical_formula_sum            'C42 H28 Fe N6 Se2'
_chemical_formula_weight         830.47
_chemical_name_systematic        '[Fe(PM-PeA)2(NCSe)2]_polymorph-II'
_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     direct
_audit_creation_date             2019-07-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-01 deposited with the CCDC.    2019-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.901(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8161(3)
_cell_length_b                   14.6779(2)
_cell_length_c                   17.1039(3)
_cell_measurement_reflns_used    13334
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.5380
_cell_measurement_theta_min      2.9630
_cell_volume                     3730.93(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.971
_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   -195.00 -15.00   1.00   20.00    -- -105.00  60.00 -36.00  180
  2  \w    -85.00 -37.00   1.00    5.00    --    5.00  48.00-108.00   48
  3  \w   -195.00 -15.00   1.00   20.00    -- -105.00  36.00 144.00  180
  4  \w   -131.00  49.00   1.00   10.00    --  -41.00  60.00-108.00  180
  5  \w   -195.00 -15.00   1.00   20.00    -- -105.00  60.00-108.00  180
  6  \w   -194.00 -15.00   1.00   20.00    -- -105.00  48.00  72.00  179
  7  \w   -105.00  48.00   1.00   10.00    --  -41.00  48.00 -72.00  153
  8  \w   -184.00-127.00   1.00   20.00    -- -105.00  12.00 -72.00   57
  9  \w   -128.00 -67.00   1.00   10.00    --  -41.00  36.00  72.00   61
 10  \w   -179.00-134.00   1.00   20.00    -- -105.00  60.00-144.00   45
 11  \w    -60.00 -15.00   1.00   20.00    -- -105.00  12.00-108.00   45
 12  \w   -190.00-145.00   1.00   20.00    -- -105.00  60.00   0.00   45
 13  \w   -158.00 -74.00   1.00   20.00    -- -105.00  60.00 -72.00   84
 14  \w   -195.00-115.00   1.00   20.00    -- -105.00  60.00  72.00   80
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0337407000
_diffrn_orient_matrix_UB_12      0.0990055000
_diffrn_orient_matrix_UB_13      0.0207241000
_diffrn_orient_matrix_UB_21      -0.0911526000
_diffrn_orient_matrix_UB_22      0.0340971000
_diffrn_orient_matrix_UB_23      -0.0733171000
_diffrn_orient_matrix_UB_31      -0.0360509000
_diffrn_orient_matrix_UB_32      0.0065318000
_diffrn_orient_matrix_UB_33      0.0677152000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27081
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.199
_diffrn_reflns_theta_min         2.974
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.771
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0993P)^2^+2.4223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6541
_reflns_number_total             7269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01137d2.cif
_cod_data_source_block           mmet29_amb-100kb
_cod_depositor_comments
'Adding full bibliography for 7234440--7234441.cif.'
_cod_original_cell_volume        3730.93(14)
_cod_database_code               7234441
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.596
_shelx_estimated_absorpt_t_min   0.160
_reflns_odcompleteness_completeness 97.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     73.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25),
  C26(H26), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C37(H37),
 C38(H38), C39(H39), C40(H40), C41(H41)
;
_shelx_res_checksum              17105
_olex2_submission_original_sample_id MMET40B
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.634
_oxdiff_exptl_absorpt_empirical_full_min 0.610