Structural phase transition in a multi-induced mononuclear Fe(II) spin-crossover complex.
Zhu, Yuan-Yuan; Liu, Chang-Wei; Yin, Ji; Meng, Zhao-Sha; Yang, Qian; Wang, Junhu; Liu, Tao; Gao, Song; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20906–20912; doi:10.1039/c5dt03216d

data_7037039
_publ_section_title
;
 Structural phase transition in a multi-induced mononuclear Fe(II)
 spin-crossover complex.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20906
_journal_page_last               20912
_journal_paper_doi               10.1039/c5dt03216d
_journal_volume                  44
_journal_year                    2015
_chemical_compound_source        no
_chemical_formula_moiety         'C30 H38 Fe N6 O4, 2(Cl O4)'
_chemical_formula_sum            'C30 H38 Cl2 Fe N6 O12'
_chemical_formula_weight         801.41
_chemical_name_common            '1a(180 K)'
_chemical_name_systematic        1032876
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-10-26 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.8634(4)
_cell_length_b                   20.0412(5)
_cell_length_c                   25.3447(8)
_cell_measurement_reflns_used    15919
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      28.1930
_cell_measurement_theta_min      3.4600
_cell_volume                     7041.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      180.01(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
  1 omega  -17.00   42.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7950  -99.0000  -90.0000 59

  2 omega   14.00   41.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7950  -99.0000  120.0000 27

  3 omega   17.00   54.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7950  -19.0000  -30.0000 37

  4 omega  -28.00   -1.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7950  -19.0000  -30.0000 27

  5 omega   34.00   65.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.7325   38.0000    0.0000 31

  6 omega  -18.00   11.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.7325  -99.0000   90.0000 29

  7 omega  -12.00   15.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.7325  -99.0000  150.0000 27
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0449043000
_diffrn_orient_matrix_UB_12      -0.0165335000
_diffrn_orient_matrix_UB_13      0.0026953000
_diffrn_orient_matrix_UB_21      -0.0075657000
_diffrn_orient_matrix_UB_22      -0.0026373000
_diffrn_orient_matrix_UB_23      0.0276296000
_diffrn_orient_matrix_UB_31      -0.0232039000
_diffrn_orient_matrix_UB_32      -0.0311935000
_diffrn_orient_matrix_UB_33      -0.0037139000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            37030
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.018
_diffrn_reflns_theta_min         3.479
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       block
_exptl_crystal_F_000             3328
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.256
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         6814
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0810P)^2^+18.4604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1688
_refine_ls_wR_factor_ref         0.1806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5628
_reflns_number_total             6814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03216d2.cif
_cod_data_source_block           1032876
_cod_depositor_comments
'Adding full bibliography for 7037038--7037042.cif.'
_cod_database_code               7037039
_chemical_oxdiff_formula         'Fe C H N O'
_shelx_estimated_absorpt_t_max   1.00000
_shelx_estimated_absorpt_t_min   0.57616
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9-O10 \\sim O9-O11 \\sim O9-O12 \\sim O10-O11 \\sim O10-O12 \\sim O11-O12
 with sigma of 0.01
 Cl2-O9 \\sim Cl2-O10 \\sim Cl2-O11 \\sim Cl2-O12
 with sigma of 0.01
 O5-O6 \\sim O5-O7 \\sim O5-O8 \\sim O6-O7 \\sim O6-O8 \\sim O7-O8
 with sigma of 0.01
 Cl1-O5 \\sim Cl1-O6 \\sim Cl1-O7 \\sim Cl1-O8
 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C12(H12A,H12B), C17(H17A,H17B), C27(H27A,H27B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C22(H22), C23(H23), C24(H24)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
;
_shelx_res_checksum              81377
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'