Reversible single-crystal to single-crystal phase transformation between a new Werner clathrate and its apohost.
Matos, Catiúcia R M O; Sanii, Rana; Wang, Shi-Qiang; Ronconi, Célia M; Zaworotko, Michael J.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 12923–12930; doi:10.1039/d1dt01839f

data_7708110
_publ_section_title
;
 Reversible single-crystal to single-crystal phase transformation between
 a new Werner clathrate and its apohost.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12923
_journal_page_last               12930
_journal_paper_doi               10.1039/d1dt01839f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C70 H40 Co N10 O8 S2, 2(C6 H5 N O2)'
_chemical_formula_sum            'C82 H50 Co N12 O12 S2'
_chemical_formula_weight         1518.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-06-30
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.06.19 svn.r9b09db45 for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-07-06 deposited with the CCDC.	2021-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.9370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.4952(6)
_cell_length_b                   24.9826(14)
_cell_length_c                   10.2664(4)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      3.07
_cell_volume                     3408.8(3)
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      101.81
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.994
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27811
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.056
_diffrn_reflns_theta_min         3.065
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       block
_exptl_crystal_F_000             1562
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5078
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0382P)^2^+3.9501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0883
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4496
_reflns_number_total             5078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01839f2.cif
_cod_data_source_block           samm-5-co-ncsnbdisordered
_cod_depositor_comments
'Adding full bibliography for 7708105--7708117.cif.'
_cod_database_code               7708110
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.926
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 C2, C9, C3, C8, C6, C7, N1, O, O1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: O1(0.5) O(0.5) C6(0.5) C7(0.5) H7(0.5) C2(0.5) H2(0.5) C9(0.5)
 H9(0.5) C3(0.5) H3(0.5) C8(0.5) H8(0.5) N1(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C009(H009), C00B(H00B), C00I(H00I), C00K(H00K), C00L(H00L), C00M(H00M),
 C00N(H00N), C00P(H00P), C00Q(H00Q), C00R(H00R), C7(H7), C2(H2), C9(H9), C3(H3),
  C8(H8)
;
_shelx_res_checksum              97468
_olex2_submission_special_instructions 'No special instructions were received'