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_7037041
_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), C2 H3 N'
_chemical_formula_sum            'C32 H41 Cl2 Fe N7 O12'
_chemical_formula_weight         842.47
_chemical_name_common            '1b(100 K)'
_chemical_name_systematic        1032885
_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
_audit_creation_date             2015-09-28
_audit_creation_method
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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                   16.9258(4)
_cell_length_b                   19.0959(5)
_cell_length_c                   22.9024(5)
_cell_measurement_reflns_used    10110
_cell_measurement_temperature    100.1(3)
_cell_measurement_theta_max      29.9710
_cell_measurement_theta_min      3.1480
_cell_volume                     7402.4(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
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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)'
_diffrn_ambient_temperature      100.1(3)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   45.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191 -178.0000   90.0000 26

  2 omega    2.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191   38.0000 -150.0000 68

  3 omega  -19.00    6.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -99.0000  -60.0000 25

  4 omega -105.00  -61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566 -178.0000  -60.0000 44

  5 omega  -19.00    6.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -99.0000 -180.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0147773000
_diffrn_orient_matrix_UB_12      0.0237233000
_diffrn_orient_matrix_UB_13      0.0211696000
_diffrn_orient_matrix_UB_21      -0.0269672000
_diffrn_orient_matrix_UB_22      0.0135881000
_diffrn_orient_matrix_UB_23      -0.0208328000
_diffrn_orient_matrix_UB_31      -0.0284776000
_diffrn_orient_matrix_UB_32      -0.0251615000
_diffrn_orient_matrix_UB_33      0.0087289000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29396
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.417
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90491
_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             3504
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/ether'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0358P)^2^+10.7559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5730
_reflns_number_total             7279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03216d2.cif
_cod_data_source_block           1032885
_cod_depositor_comments
'Adding full bibliography for 7037038--7037042.cif.'
_cod_database_code               7037041
_chemical_oxdiff_formula         'C H O N Cl Fe'
_shelx_estimated_absorpt_t_max   1.00000
_shelx_estimated_absorpt_t_min   0.90491
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C12(H12A,H12B), C19(H19A,H19B), C27(H27A,H27B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C22(H22), C23(H23), C24(H24)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              95357
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'