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_7708107
_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 N10 Ni O8 S2, 2(C6 H5 N O2)'
_chemical_formula_sum            'C82 H50 N12 Ni O12 S2'
_chemical_formula_weight         1518.17
_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                 120.7810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.3777(7)
_cell_length_b                   24.8980(10)
_cell_length_c                   10.2613(4)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.75
_cell_volume                     3375.3(2)
_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      100.85
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_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       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25133
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.147
_diffrn_reflns_theta_min         2.749
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       block
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5051
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0406P)^2^+5.5909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4329
_reflns_number_total             5051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01839f2.cif
_cod_data_source_block           samm-5-ni-ncsnbdisordered
_cod_depositor_comments
'Adding full bibliography for 7708105--7708117.cif.'
_cod_database_code               7708107
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.919
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O00V-N00C \\sim O00U-N00C
 with sigma of 0.001
 O00V-C00V \\sim C00V-O00U
 with sigma of 0.001
3. Restrained planarity
 N00C, C00V, O00U, O00V, C00U, C1, C00P, H00U, C00Q, H1, H00P, C4, H00Q, H4
 with sigma of 0.001
4. Others
 Fixed Sof: N00C(0.5) C00V(0.5) C00U(0.5) H00U(0.5) C00P(0.5) H00P(0.5)
 C4(0.5) H4(0.5) C00Q(0.5) H00Q(0.5) C1(0.5) H1(0.5) O00U(0.5) O00V(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C008(H008), C00B(H00B), C00D(H00D), C00H(H00H), C00K(H00K), C00M(H00M),
 C00N(H00N), C00O(H00O), C00R(H00R), C00S(H00S), C00U(H00U), C00P(H00P), C4(H4),
  C00Q(H00Q), C1(H1)
5.b Fitted hexagon refined as free rotating group:
 C00V(C00U,C00P,C4,C00Q,C1)
;
_shelx_res_checksum              43218
_olex2_submission_special_instructions 'No special instructions were received'