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_7708116
_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(C8 H10)'
_chemical_formula_sum            'C86 H60 Co N10 O8 S2'
_chemical_formula_weight         1484.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-05 deposited with the CCDC.	2021-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                110.5340(10)
_cell_angle_beta                 97.7010(10)
_cell_angle_gamma                93.6120(10)
_cell_formula_units_Z            1
_cell_length_a                   8.9800(2)
_cell_length_b                   13.9351(3)
_cell_length_c                   15.8237(3)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.63
_cell_volume                     1824.64(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      299.99
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0283
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31414
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         2.487
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0518 before and 0.0420 after correction. The Ratio of minimum to maximum transmission is 0.9581. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       needles
_exptl_crystal_F_000             769
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         6441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0437P)^2^+0.8955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5431
_reflns_number_total             6441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01839f2.cif
_cod_data_source_block           SAMM-5-Co-NCSOX
_cod_depositor_comments
'Adding full bibliography for 7708105--7708117.cif.'
_cod_database_code               7708116
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.894
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00F(H00F), C00I(H00I), C00S(H00S), C00V(H00V), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C012(H012),
 C013(H013), C014(H014), C015(H015), C016(H016), C017(H017), C018(H018),
 C019(H019), C01B(H01B), C01D(H01D), C01E(H01E), C01F(H01F), C01H(H01H)
2.b Idealised Me refined as rotating group:
 C01G(H01A,H01C,H01G), C01I(H01I,H01J,H01K)
;
_shelx_res_checksum              70157
_olex2_submission_special_instructions 'No special instructions were received'