Water molecule induced reversible single-crystal-to-single-crystal transformation between two trinuclear Fe(ii) complexes with different spin crossover behaviour.
Chen, Wen-Bin; Chen, Yan-Cong; Yang, Meng; Tong, Ming-Liang; Dong, Wen; Dalton transactions (Cambridge, England : 2003) 47 (2018) 4307–4314; doi:10.1039/c8dt00318a

data_1548935
_publ_section_title
;
 Water molecule induced reversible single-crystal-to-single-crystal
 transformation between two trinuclear Fe(ii) complexes with different
 spin crossover behaviour.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4307
_journal_page_last               4314
_journal_paper_doi               10.1039/c8dt00318a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C17 H26 Fe3 N29 O S5, C N S'
_chemical_formula_sum            'C18 H26 Fe3 N30 O S6'
_chemical_formula_weight         1038.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-09 deposited with the CCDC.
2018-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.972(4)
_cell_length_b                   11.475(6)
_cell_length_c                   31.878(11)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.666
_cell_measurement_theta_min      2.561
_cell_volume                     4014(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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_temperature      150.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            40781
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.518
_diffrn_reflns_theta_max         25.518
_diffrn_reflns_theta_min         2.556
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.446
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0791 before and 0.0696 after correction. The Ratio of minimum to maximum transmission is 0.8312. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Flack x determined using 2137 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.042(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         7423
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+26.4198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                6008
_reflns_number_total             7423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00318a2.cif
_cod_data_source_block           d
_cod_depositor_comments
'Adding full bibliography for 1548933--1548938.cif.'
_cod_database_code               1548935
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.735
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N4) \\sim Ueq, Uanis(N23) \\sim Ueq, Uanis(N24) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(N3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Riding coordinates:
 N16(H16A,H16B), O1(H1A,H1B)
3.b Rotating group:
 N4(H4A,H4B), N8(H8A,H8B), N12(H12A,H12B), N20(H20A,H20B), N24(H24A,H24B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'