Symmetry breaking above room temperature in an Fe(ii) spin crossover complex with an N4O2 donor set.
Phonsri, Wasinee; Davies, Casey G.; Jameson, Guy N. L.; Moubaraki, Boujemaa; Ward, Jas S.; Kruger, Paul E.; Chastanet, Guillaume; Murray, Keith S.; Chemical communications (Cambridge, England) 53 (2017) 1374–1377; doi:10.1039/c6cc10040f

data_7119365
_publ_section_title
;
 Symmetry breaking above room temperature in an Fe(ii) spin crossover
 complex with an N4O2 donor set.
;
_journal_issue                   8
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1374
_journal_page_last               1377
_journal_paper_doi               10.1039/c6cc10040f
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C32 H20 Cl2 Fe N4 O2'
_chemical_formula_sum            'C32 H20 Cl2 Fe N4 O2'
_chemical_formula_weight         619.27
_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
_audit_creation_date             2016-05-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-25 deposited with the CCDC.
2017-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.2672(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2113(2)
_cell_length_b                   12.9889(2)
_cell_length_c                   19.6876(4)
_cell_measurement_reflns_used    6641
_cell_measurement_temperature    298.01(10)
_cell_measurement_theta_max      73.9580
_cell_measurement_theta_min      4.7700
_cell_volume                     2606.99(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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   -107.00 -16.00   1.00   10.00    --  -38.50 -57.00-120.00   91
  2  \w    -64.00  30.00   1.00   10.00    --  -38.50  57.00  30.00   94
  3  \w    -13.00  25.00   1.00   10.00    --  -38.50  37.00-180.00   38
  4  \w     36.00  62.00   1.00   10.00    --   42.63-125.00  60.00   26
  5  \w    -24.00  72.00   1.00   10.00    --   42.63 -77.00 120.00   96
  6  \w     37.00  89.00   1.00   40.00    --  105.36 -30.00   0.00   52
  7  \w     34.00 108.00   1.00   40.00    --  105.36 -94.00-180.00   74
  8  \w     66.00  92.00   1.00   40.00    --  105.36 -49.00-128.00   26
  9  \w     49.00 109.00   1.00   40.00    --  105.36 -94.00 -90.00   60
 10  \w     27.00 142.00   1.00   40.00    --  105.36 -15.00  90.00  115
 11  \w     95.00 171.00   1.00   40.00    --  105.36 125.00-120.00   76
 12  \w     55.00  80.00   1.00   40.00    --  105.36 -30.00  60.00   25
 13  \w     32.00  91.00   1.00   40.00    --  105.36 -30.00 -90.00   59
 14  \w     44.00  81.00   1.00   40.00    --  105.36 -45.00 -30.00   37
 15  \w     49.00  95.00   1.00   40.00    --  105.36 -94.00   0.00   46
 16  \w     32.00  91.00   1.00   40.00    --  105.36 -30.00-150.00   59
 17  \w     49.00  97.00   1.00   40.00    --  105.36 -45.00 150.00   48
 18  \w     48.00  73.00   1.00   40.00    --  105.36 -30.00  30.00   25
 19  \w     61.00 117.00   1.00   40.00    --  105.36-125.00 120.00   56
 20  \w    102.00 127.00   1.00   40.00    --  105.36  77.00   0.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0203715000
_diffrn_orient_matrix_UB_12      -0.1095711000
_diffrn_orient_matrix_UB_13      0.0274735000
_diffrn_orient_matrix_UB_21      -0.1359585000
_diffrn_orient_matrix_UB_22      -0.0045191000
_diffrn_orient_matrix_UB_23      -0.0380957000
_diffrn_orient_matrix_UB_31      0.0628519000
_diffrn_orient_matrix_UB_32      -0.0451928000
_diffrn_orient_matrix_UB_33      -0.0627114000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18456
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.943
_diffrn_reflns_theta_min         4.080
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.854
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0609P)^2^+1.0651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1215
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4326
_reflns_number_total             5228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc10040f2.cif
_cod_data_source_block           WS74-298K_scale
_cod_depositor_comments
'Adding full bibliography for 7119364--7119369.cif.'
_cod_original_cell_volume        2606.99(9)
_cod_database_code               7119365
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C18(H18), C19(H19), C21(H21), C23(H23), C25(H25), C26(H26),
  C27(H27), C29(H29), C30(H30), C31(H31)
;
_shelx_res_checksum              76468
_ins_header
;
TITL WS74-298(2)_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  10.211290  12.988883  19.687624  90.0000  93.2672  90.0000
ZERR    4.00   0.000211   0.000245   0.000371   0.0000   0.0018   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H N O Cl Fe
UNIT 128.00 80.00 16.00 8.00 8.00 4.00
TREF
HKLF 4
END
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.976
_oxdiff_exptl_absorpt_empirical_full_min 0.693