Exploiting the equilibrium dynamics in the self-assembly of inorganic macrocycles based upon polyoxothiometalate building blocks.
Zang, Hongying; Surman, Andrew; Long, Deliang; Cronin, Leroy; Miras, Haralampos N.; Chemical communications (Cambridge, England) 52 (2016) 9109–9112; doi:10.1039/c6cc01041e

data_7118898
_publ_section_title
;
 Exploiting the equilibrium dynamics in the self-assembly of inorganic
 macrocycles based upon polyoxothiometalate building blocks.
;
_journal_issue                   58
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9109
_journal_page_last               9112
_journal_paper_doi               10.1039/c6cc01041e
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C12 H96 K3 Mo16 N O74 S16'
_chemical_formula_weight         3604.19
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'F map'
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-02-01 deposited with the CCDC.
2016-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.634(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
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_cell_length_c                   23.3822(11)
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      2.30
_cell_volume                     5151.2(4)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        Apex2
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex II Quasar'
_diffrn_measurement_method       '\w & \p scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34709
_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         25.998
_diffrn_reflns_theta_min         1.838
_diffrn_source                   '30 W microfocus sealed tube, Quazar\"i?1/2'
_exptl_absorpt_coefficient_mu    2.418
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.324
_exptl_crystal_density_method    none
_exptl_crystal_description       block
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_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.83
_refine_diff_density_min         -1.19
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_refine_ls_extinction_coef       0.00013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0693P)^2^+109.8552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4867
_reflns_number_total             5319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc01041e2.cif
_cod_data_source_block           hz3482
_cod_depositor_comments
;Adding full bibliography for 7118898--7118899.cif.

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct method' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               7118898
_shelx_estimated_absorpt_t_min   0.830
_shelx_estimated_absorpt_t_max   0.868
_shelxl_version_number           2013-4