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_7708114
_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
;
2021-07-07 deposited with the CCDC.	2021-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.211(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.6422(16)
_cell_length_b                   24.988(3)
_cell_length_c                   10.2512(11)
_cell_measurement_reflns_used    6199
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.93
_cell_measurement_theta_min      2.71
_cell_volume                     3426.9(7)
_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      110.64
_diffrn_measured_fraction_theta_full 0.998
_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  0.0853
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14491
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.991
_diffrn_reflns_theta_max         24.991
_diffrn_reflns_theta_min         2.838
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       prism
_exptl_crystal_F_000             1562
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.239
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3096
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0391P)^2^+7.1996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1365
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2394
_reflns_number_total             3096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01839f2.cif
_cod_data_source_block           samm-5-co-ncsnbaftersoaking
_cod_depositor_comments
'Adding full bibliography for 7708105--7708117.cif.'
_cod_original_cell_volume        3426.9(6)
_cod_database_code               7708114
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.890
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C00A-C00G = C00G-C00L = C00L-C00N = C00N-C00M = C00M-C00D = C00D-C00A
 1.39 with sigma of 0.01
 C00H-C00K = C00K-C00P = C00P-C00Q = C00Q-C00M = C00M-C00D = C00D-C00H
 1.39 with sigma of 0.01
 C5-C7 = C7-C3 = C3-CXF = CXF-C2 = C2-C6 = C6-C5
 1.39 with sigma of 0.01
 C5-C3 \\sim C7-CXF \\sim C3-C2 \\sim CXF-C6 \\sim C2-C5 \\sim C6-C7
 with sigma of 0.02
 C00A-C00L \\sim C00G-C00N \\sim C00L-C00M \\sim C00N-C00D \\sim C00M-C00A
\\sim C00D-C00G
 with sigma of 0.02
 C00H-C00P \\sim C00K-C00Q \\sim C00P-C00M \\sim C00Q-C00D \\sim C00M-C00H
\\sim C00D-C00K
 with sigma of 0.02
3. Restrained planarity
 C00A, C00G, C00L, C00N, C00M, C00D
 with sigma of 0.1
 C5, C7, C3, CXF, C2, C6
 with sigma of 0.1
 C00H, C00K, C00P, C00Q, C00M, C00D
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 N1, C5, O1, O2, C6, C7, C2, C3, CXF
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: N1(0.5) C2(0.5) H2(0.5) C6(0.5) H6(0.5) C5(0.5) C7(0.5) H7(0.5)
 C3(0.5) H3(0.5) CXF(0.5) HXF(0.5) O1(0.5) O2(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C008(H008), C00F(H00F), C00G(H00G), C00I(H00I), C00J(H00J), C00K(H00K),
 C00L(H00L), C00N(H00N), C00P(H00P), C00Q(H00Q), C2(H2), C6(H6), C7(H7), C3(H3),
  CXF(HXF)
;
_shelx_res_checksum              93728
_olex2_submission_special_instructions 'No special instructions were received'