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_7119364
_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             2016-05-27
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
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2016-07-25 deposited with the CCDC.
2017-01-06 downloaded from the CCDC.
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
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  1 omega  -87.00  -29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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  2 omega -108.00   -8.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega  -44.00  -18.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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  4 omega  -92.00   -2.00   1.0000   10.0000
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  5 omega   27.00   90.00   1.0000   10.0000
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  6 omega  131.00  163.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega   37.00   99.00   1.0000   40.0000
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  8 omega   38.00   85.00   1.0000   40.0000
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  9 omega   33.00   83.00   1.0000   40.0000
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 10 omega   65.00   95.00   1.0000   40.0000
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 11 omega   26.00  102.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
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 12 omega   39.00   88.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3576  -45.0000  -90.0000 49

 13 omega   60.00  119.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3576 -125.0000  -60.0000 59

 14 omega   42.00   82.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
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 15 omega   27.00   95.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3576  -94.0000 -180.0000 68

 16 omega   51.00  107.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3576  -94.0000  -60.0000 56

 17 omega   28.00   54.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3576  -94.0000   90.0000 26

 18 omega   84.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3576  -94.0000   90.0000 25

 19 omega   21.00  172.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3576    0.0000 -120.0000 151
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_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      0.0196284000
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_diffrn_orient_matrix_UB_33      0.0643957000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_number            17188
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_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.041
_diffrn_reflns_theta_min         4.123
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.028
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_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
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    1.618
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_exptl_crystal_F_000             1264
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_refine_diff_density_max         0.504
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+1.3920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1186
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4525
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc10040f2.cif
_cod_data_source_block           WS74-100K_scale
_cod_depositor_comments
'Adding full bibliography for 7119364--7119369.cif.'
_cod_original_cell_volume        2542.30(9)
_cod_database_code               7119364
_shelxl_version_number           2014/6
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_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              1477
_ins_header
;
TITL WS74-100K_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  10.204382  12.883501  19.377646  90.0000  93.6752  90.0000
ZERR    4.00   0.000231   0.000245   0.000376   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'