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_7037042
_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(173 K)'
_chemical_name_systematic        1410363
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-10-26 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.79(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.909(3)
_cell_length_b                   20.024(4)
_cell_length_c                   25.221(5)
_cell_measurement_reflns_used    18527
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      2.3757
_cell_volume                     7021(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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    ????
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.0495
              2theta: -20.0959
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.0495
              2theta: -20.0959
scan:
    Number of images: 200
               Slice: -100.0000 - 0.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 45.0495
              2theta: -20.0959
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0699
_diffrn_orient_matrix_UB_12      0.0122
_diffrn_orient_matrix_UB_13      0.0117
_diffrn_orient_matrix_UB_21      -0.0076
_diffrn_orient_matrix_UB_22      -0.0039
_diffrn_orient_matrix_UB_23      0.0492
_diffrn_orient_matrix_UB_31      0.0084
_diffrn_orient_matrix_UB_32      -0.0387
_diffrn_orient_matrix_UB_33      -0.0018
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.1215
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       16
_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       -1
_diffrn_reflns_number            12609
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.584
_diffrn_reflns_theta_min         2.507
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           90.0000
_diffrn_source_power             4.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8256
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3328
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.5000
_exptl_crystal_size_mid          0.4600
_exptl_crystal_size_min          0.1800
_refine_diff_density_max         1.759
_refine_diff_density_min         -2.076
_refine_diff_density_rms         0.191
_refine_ls_extinction_coef       0.0047(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.359
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         12609
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.370
_refine_ls_R_factor_all          0.1918
_refine_ls_R_factor_gt           0.1582
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4041
_refine_ls_wR_factor_ref         0.4351
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7753
_reflns_number_total             12609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03216d2.cif
_cod_data_source_block           1410363
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7037038--7037042.cif.

2017-03-01
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C30 H38 Fe N6 O4), 4(Cl O4)'
_cod_original_formula_sum        'C60 H76 Cl4 Fe2 N12 O24'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1602.82
_cod_database_code               7037042
_diffrn_number_total             15994
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.63 0.37
2. 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
3. Restrained distances
 O21-O22 \\sim O22-O23 \\sim O23-O24 \\sim O24-O21
 with sigma of 0.01
 Cl4-O21 \\sim Cl4-O22 \\sim Cl4-O23 \\sim Cl4-O24
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O21) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O24)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C12(H12A,H12B), C19(H19A,H19B), C27(H27A,H27B), C34(H34A,H34B),
 C42(H42A,H42B), C49(H49A,H49B), C57(H57A,H57B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C22(H22), C23(H23), C24(H24), C37(H37), C38(H38),
 C39(H39), C52(H52), C53(H53), C54(H54)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C)
;
_shelx_res_checksum              4778
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'