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_7119369
_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             2016-05-21
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Olex2 1.2
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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                 94.140(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_c                   19.5205(6)
_cell_measurement_reflns_used    5558
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_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)
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_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)
;
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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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_diffrn_measurement_details
;
  1 omega -116.00  -11.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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  2 omega  -46.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega  -18.00   26.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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  4 omega   17.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.6255   77.0000   60.0000 27

  5 omega   43.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.6255 -125.0000   90.0000 51

  6 omega   23.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.6255 -125.0000  -60.0000 64

  7 omega   41.00   94.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -150.0000 53

  8 omega  139.00  176.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000 -120.0000 37

  9 omega   50.00   93.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -30.0000 43

 10 omega   49.00   88.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  120.0000 39

 11 omega   44.00  122.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  120.0000 78

 12 omega  146.00  172.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  150.0000 26

 13 omega   68.00  107.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -90.0000 39

 14 omega   78.00  115.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   30.0000 37

 15 omega   47.00  115.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -90.0000 68

 16 omega   41.00   99.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -90.0000 58

 17 omega  105.00  131.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000   90.0000 26

 18 omega   41.00   90.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   90.0000 49

 19 omega   56.00   89.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   30.0000 33

 20 omega  102.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   30.0000 76

 21 omega   49.00  106.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 57

 22 omega   86.00  177.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000  -30.0000 91
;
_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      -0.0192098000
_diffrn_orient_matrix_UB_12      -0.1082323000
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_diffrn_orient_matrix_UB_21      -0.1354134000
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_diffrn_orient_matrix_UB_23      -0.0376323000
_diffrn_orient_matrix_UB_31      0.0581554000
_diffrn_orient_matrix_UB_32      -0.0446400000
_diffrn_orient_matrix_UB_33      -0.0638235000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19362
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_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.952
_diffrn_reflns_theta_min         4.056
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.712
_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    1.545
_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         0.388
_refine_diff_density_min         -0.397
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         5544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0687P)^2^+0.7669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1431
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4180
_reflns_number_total             5544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc10040f2.cif
_cod_data_source_block           WS74-330K_scale
_cod_depositor_comments
'Adding full bibliography for 7119364--7119369.cif.'
_cod_database_code               7119369
_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              78775
_ins_header
;
TITL WS74-330K_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  10.396951  13.151326  19.520531  90.0000  94.1403  90.0000
ZERR    4.00   0.000361   0.000383   0.000623   0.0000   0.0030   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'