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_7708108
_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           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-04-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-08 deposited with the CCDC.	2021-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.149(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2636(4)
_cell_length_b                   24.8917(10)
_cell_length_c                   13.4739(6)
_cell_measurement_reflns_used    7583
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.83
_cell_volume                     3388.4(2)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      104.31
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0760
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            51779
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.313
_diffrn_reflns_theta_min         2.450
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.427
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       prism
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         8399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0553P)^2^+1.0783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5787
_reflns_number_total             8399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01839f2.cif
_cod_data_source_block           SAMM-5-Ni-NCSNB
_cod_depositor_comments
'Adding full bibliography for 7708105--7708117.cif.'
_cod_database_code               7708108
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.935
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00I(H00I), C00J(H00J), C00L(H00L), C00M(H00M), C00R(H00R),
 C00S(H00S), C00V(H00V), C00W(H00W), C00Z(H00Z), C011(H011), C012(H012),
 C013(H013), C016(H016), C018(H018), C019(H019), C01A(H01A), C01B(H01B),
 C01C(H01C), C01E(H01E), C01F(H01F), C01G(H01G), C01H(H01H), C01I(H01I),
 C01J(H01J)
;
_shelx_res_checksum              8684
_olex2_submission_special_instructions 'No special instructions were received'