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_7119366
_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      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-22
_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                90.988(3)
_cell_angle_beta                 93.801(3)
_cell_angle_gamma                90.596(3)
_cell_formula_units_Z            4
_cell_length_a                   10.2926(5)
_cell_length_b                   13.0726(5)
_cell_length_c                   19.6371(8)
_cell_measurement_reflns_used    5032
_cell_measurement_temperature    308.01(10)
_cell_measurement_theta_max      75.3780
_cell_measurement_theta_min      4.5140
_cell_volume                     2635.8(2)
_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)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      308.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_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    -91.00 -42.00   1.00   10.00    --  -38.50 125.00 120.00   49
  2  \w    -46.00  31.00   1.00   10.00    --  -38.50  37.00-150.00   77
  3  \w   -110.00 -51.00   1.00   10.00    --  -38.50 -37.00  90.00   59
  4  \w   -109.00 -10.00   1.00   10.00    --  -38.50 -77.00  30.00   99
  5  \w    -27.00  23.00   1.00   10.00    --   42.63 -48.00-127.00   50
  6  \w      1.00  58.00   1.00   10.00    --   42.63 -99.00 -30.00   57
  7  \w     95.00 121.00   1.00   40.00    --  111.00-125.00-150.00   26
  8  \w     46.00  75.00   1.00   40.00    --  111.00-125.00-150.00   29
  9  \w     87.00 121.00   1.00   40.00    --  111.00 -61.00 -90.00   34
 10  \w     38.00  88.00   1.00   40.00    --  111.00 -30.00 -30.00   50
 11  \w     37.00 107.00   1.00   40.00    --  111.00 -94.00-120.00   70
 12  \w     40.00  75.00   1.00   40.00    --  111.00 -30.00 -90.00   35
 13  \w     59.00 118.00   1.00   40.00    --  111.00-125.00  90.00   59
 14  \w     90.00 159.00   1.00   40.00    --  111.00  30.00-120.00   69
 15  \w     38.00  74.00   1.00   40.00    --  111.00 -30.00 120.00   36
 16  \w     42.00  94.00   1.00   40.00    --  111.00 -45.00-150.00   52
 17  \w    141.00 173.00   1.00   40.00    --  111.00  45.00 150.00   32
 18  \w     89.00 137.00   1.00   40.00    --  111.00  45.00 150.00   48
 19  \w     60.00 131.00   1.00   40.00    --  111.00 -77.00  90.00   71
 20  \w     83.00 109.00   1.00   40.00    --  111.00 -94.00 -60.00   26
 21  \w    123.00 152.00   1.00   40.00    --  111.00  30.00 -60.00   29
 22  \w     42.00  97.00   1.00   40.00    --  111.00 -45.00  30.00   55
 23  \w     95.00 122.00   1.00   40.00    --  111.00  15.00 -90.00   27
 24  \w    137.00 172.00   1.00   40.00    --  111.00  15.00 -90.00   35
 25  \w     53.00  84.00   1.00   40.00    --  111.00 -61.00 -90.00   31
;
_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      -0.0200646000
_diffrn_orient_matrix_UB_12      -0.1082521000
_diffrn_orient_matrix_UB_13      0.0275610000
_diffrn_orient_matrix_UB_21      -0.1362544000
_diffrn_orient_matrix_UB_22      -0.0057635000
_diffrn_orient_matrix_UB_23      -0.0374865000
_diffrn_orient_matrix_UB_31      0.0594748000
_diffrn_orient_matrix_UB_32      -0.0462820000
_diffrn_orient_matrix_UB_33      -0.0633953000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19835
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.727
_diffrn_reflns_theta_min         3.382
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.779
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49533
_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    1.561
_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         1.010
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         10745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0655
_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^)+(0.1081P)^2^+0.3048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1744
_refine_ls_wR_factor_ref         0.2002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7485
_reflns_number_total             10745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc10040f2.cif
_cod_data_source_block           WS74-308K_scale
_cod_depositor_comments
'Adding full bibliography for 7119364--7119369.cif.'
_cod_original_cell_volume        2635.81(19)
_cod_database_code               7119366
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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), C52(H52), C53(H53), C55(H55),
 C57(H57), C59(H59), C60(H60), C61(H61), C63(H63), C64(H64), C65(H65), C68(H68),
  C69(H69), C71(H71), C73(H73), C75(H75), C76(H76), C77(H77), C79(H79),
 C80(H80), C81(H81)
;
_shelx_res_checksum              70895
_ins_header
;
TITL WS74-308K_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  10.292577  13.072625  19.637113  90.9879  93.8009  90.5963
ZERR    4.00   0.000454   0.000532   0.000759   0.0032   0.0034   0.0034
LATT  1
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 1.696
_oxdiff_exptl_absorpt_empirical_full_min 0.729