Exploring Structural Complexity in the Discovery and Self-Assembly of a Family of Nanoscale Chalcoxides from {Se8Mo36} to {Se26Mo68}
Cronin, Lee; Zang, Hong-Ying; Purcell, Jamie; Long, Deliang; Miras, Haralampos N.; Chem. Commun.  (2017) –; doi:10.1039/C7CC04398H

data_7120385
_publ_section_title
;
 Exploring Structural Complexity in the Discovery and Self-Assembly of a
 Family of Nanoscale Chalcoxides from {Se8Mo36} to {Se26Mo68}
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04398H
_journal_year                    2017
_chemical_formula_sum            'C48 H276 K30 Mo68 N4 Na2 O310 S68 Se26'
_chemical_formula_weight         17846.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-28 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                102.220(2)
_cell_angle_beta                 100.029(2)
_cell_angle_gamma                95.818(2)
_cell_formula_units_Z            1
_cell_length_a                   20.3775(7)
_cell_length_b                   21.0899(7)
_cell_length_c                   30.3195(12)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.1
_cell_measurement_theta_min      2.22
_cell_volume                     12410.2(8)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        Apex2
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex II Quasar'
_diffrn_measurement_method       '\w & \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1076
_diffrn_reflns_av_unetI/netI     0.1103
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            129811
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        22.710
_diffrn_reflns_theta_max         22.710
_diffrn_reflns_theta_min         1.077
_diffrn_source                   '1uS Microfocus x-ray'
_exptl_absorpt_coefficient_mu    4.187
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.388
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             8492
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.66
_refine_diff_density_min         -0.96
_refine_diff_density_rms         0.24
_refine_ls_extinction_coef       0.000116(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2536
_refine_ls_number_reflns         33181
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1331
_refine_ls_R_factor_gt           0.0660
_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^)+(0.0841P)^2^+318.5470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1640
_refine_ls_wR_factor_ref         0.2122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19372
_reflns_number_total             33181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04398h2.cif
_cod_data_source_block           hz4311
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7120385
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.680
_shelx_estimated_absorpt_t_max   0.850
_shelx_res_checksum              1904