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_7119368
_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
_audit_creation_date             2016-05-23
_audit_creation_method
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
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_audit_update_record
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2016-07-25 deposited with the CCDC.
2017-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.034(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3632(3)
_cell_length_b                   13.1281(3)
_cell_length_c                   19.5466(5)
_cell_measurement_reflns_used    5591
_cell_measurement_temperature    318.01(10)
_cell_measurement_theta_max      76.2430
_cell_measurement_theta_min      4.5370
_cell_volume                     2652.71(12)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_ambient_environment      air
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_diffrn_measurement_details
;
  1 omega -109.00   -8.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -77.0000  -30.0000 101

  2 omega  -57.00   28.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000  150.0000 85

  3 omega   -6.00   20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000  120.0000 26

  4 omega  -49.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   37.0000  -90.0000 82

  5 omega  -64.00  -37.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000  120.0000 27

  6 omega  -15.00   29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   48.0000   20.0000 44

  7 omega   42.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.6255 -125.0000  -90.0000 54

  8 omega   49.00   74.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -90.0000 25

  9 omega   89.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -180.0000 89

 10 omega   47.00   81.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  150.0000 34

 11 omega   45.00  117.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   60.0000 72

 12 omega   45.00  132.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000   30.0000 87

 13 omega   46.00   91.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   60.0000 45

 14 omega  146.00  176.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000   90.0000 30

 15 omega   95.00  134.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000   90.0000 39

 16 omega   43.00   80.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  150.0000 37

 17 omega   44.00   75.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   30.0000 31

 18 omega   47.00   90.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -180.0000 43

 19 omega   90.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   90.0000 88

 20 omega   80.00  122.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -150.0000 42

 21 omega   53.00   97.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -48.0000 -127.0000 44

 22 omega   38.00   63.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -60.0000 25

 23 omega   48.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 61
;
_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_UB_11      -0.0193609000
_diffrn_orient_matrix_UB_12      -0.1083695000
_diffrn_orient_matrix_UB_13      0.0277556000
_diffrn_orient_matrix_UB_21      -0.1357066000
_diffrn_orient_matrix_UB_22      -0.0039970000
_diffrn_orient_matrix_UB_23      -0.0375436000
_diffrn_orient_matrix_UB_31      0.0584705000
_diffrn_orient_matrix_UB_32      -0.0448885000
_diffrn_orient_matrix_UB_33      -0.0637244000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19430
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.689
_diffrn_reflns_theta_min         4.060
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.736
_exptl_absorpt_correction_T_max  1.00000
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_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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    1.551
_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         0.333
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0591P)^2^+0.8769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1314
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4159
_reflns_number_total             5512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc10040f2.cif
_cod_data_source_block           WS74-318K_scale
_cod_depositor_comments
'Adding full bibliography for 7119364--7119369.cif.'
_cod_database_code               7119368
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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              60564
_ins_header
;
TITL WS74-318K_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  10.363220  13.128064  19.546624  90.0000  94.0343  90.0000
ZERR    4.00   0.000290   0.000320   0.000535   0.0000   0.0025   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'