Reversible Crystal-to-Crystal Transformation from Trinuclear Cluster to 1D Chain and Corresponding Spin Crossover (SCO) Behaviour Change
Chen, Wen-Bin; Leng, Ji-Dong; Wang, Zi-Zhou; Chen, Yan-Cong; Miao, Yu; Tong, Mingliang; Dong, Wen; Chem. Commun.  (2017) –; doi:10.1039/C7CC04036A

data_7120303
_publ_section_title
;
 Reversible Crystal-to-Crystal Transformation from Trinuclear Cluster to
 1D Chain and Corresponding Spin Crossover (SCO) Behaviour Change
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04036A
_journal_year                    2017
_chemical_formula_moiety         'C17 H26 Fe3 N29 O S5, C N S, 4(H2 O)'
_chemical_formula_sum            'C18 H34 Fe3 N30 O5 S6'
_chemical_formula_weight         1110.66
_chemical_name_systematic        '[Fe3(NH2-trz)6(SCN)5(H2O)] (SCN).4H2O'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-05-24 deposited with the CCDC.
2017-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.2580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5773(4)
_cell_length_b                   23.0123(9)
_cell_length_c                   16.4758(7)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.22
_cell_measurement_theta_min      2.53
_cell_volume                     4272.5(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      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0730
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            61397
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         2.530
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.371
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1032 before and 0.0546 after correction. The Ratio of minimum to maximum transmission is 0.9284. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       block
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.327
_refine_diff_density_min         -1.869
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         9796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0749P)^2^+21.5215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7281
_reflns_number_total             9796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04036a2.cif
_cod_data_source_block           a
_cod_database_code               7120303
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.821
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2A,H2B} of O2, {H3A,H3B} of O3, {H4C,H4D} of O4, {H5A,
  H5B} of O5, All N(H,H) groups
 At 1.5 times of:
  {H1A,H1B} of O1
2.a Riding coordinates:
 N4(H4A,H4B), N8(H8A,H8B), N12(H12A,H12B), N16(H16A,H16B), N20(H20A,H20B),
 N24(H24A,H24B), O1(H1A,H1B), O2(H2A,H2B), O3(H3A,H3B), O4(H4C,H4D), O5(H5A,H5B)
2.b 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)
;
_shelx_res_checksum              31405
_olex2_submission_special_instructions 'No special instructions were received'