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_7037040
_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(100 K)'
_chemical_name_systematic        1032884
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-10-07
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.09.07 svn.r3215 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2015-10-26 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.395(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.8080(7)
_cell_length_b                   19.7339(9)
_cell_length_c                   25.0603(12)
_cell_measurement_reflns_used    10055
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      27.9130
_cell_measurement_theta_min      3.0410
_cell_volume                     6822.6(6)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
  1 omega  -61.00  -29.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7950  -38.0000    0.0000 32

  2 omega  -23.00    4.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7950   19.0000 -180.0000 27

  3 omega  -36.00   -4.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.7325   38.0000 -150.0000 32

  4 omega  -34.00   -7.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.7325  105.0000  153.0000 27

  5 omega   41.00   66.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.7325   38.0000 -150.0000 25

  6 omega   27.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.7325   57.0000 -120.0000 32

  7 omega  -19.00   32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.7325  -99.0000 -120.0000 51
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12683
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.953
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56507
_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    1.560
_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          0.2
_refine_diff_density_max         2.335
_refine_diff_density_min         -1.994
_refine_diff_density_rms         0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         12683
_refine_ls_number_restraints     960
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.1918
_refine_ls_R_factor_gt           0.1769
_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^)+(0.0455P)^2^+252.3126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4129
_refine_ls_wR_factor_ref         0.4202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10662
_reflns_number_total             12683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03216d2.cif
_cod_data_source_block           1032884
_cod_depositor_comments
;
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               7037040
_chemical_oxdiff_formula         'C H O N Cl Fe'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.58(9) 0.37(3) 0.05(8)
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. Rigid body (RIGU) restrains
 Cl4, O22, O23, O21, O24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O11, O9, O12, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2, O15, O14, O16, O13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38, Fe2, N12, N11, N10, N8, N9, N7, C56, C58, C51, C55, C50, C48, C36, C40,
 C43, C41, C35, C33, O8, C57, C60, C59, C52, C54, O7, C49, C46, C47, C37, C39,
 C44, C42, C45, O6, O5, C34, C32, C31, C53
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O2, Fe1, N5, N1, N2, N6, N3, N4, C25, C21, C3, C5, C6, C10, C26, C28, C11,
 C13, C18, C20, C24, C22, C1, C4, C2, O1, C7, C9, O4, C27, C29, C30, C15, C14,
 C12, C16, C17, C19, O3, C23, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C49(H49A,H49B), C57(H57A,H57B), C4(H4A,H4B), C34(H34A,H34B),
 C42(H42A,H42B), C12(H12A,H12B), C19(H19A,H19B)
4.b Aromatic/amide H refined with riding coordinates:
 C52(H52), C37(H37), C23(H23), C8(H8), C54(H54), C38(H38), C9(H9), C24(H24),
 C39(H39), C22(H22), C53(H53), C7(H7)
4.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C1(H1A,H1B,H1C), C44(H44A,H44B,H44C), C60(H60A,H60B,
 H60C), C59(H59A,H59B,H59C), C16(H16A,H16B,H16C), C14(H14A,H14B,H14C), C2(H2A,
 H2B,H2C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C32(H32A,H32B,
 H32C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              83857
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'