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_7120384
_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 H192 K28 Mo56 N4 O236 S56 Se20'
_chemical_formula_weight         14444.04
_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                107.720(3)
_cell_angle_beta                 101.595(3)
_cell_angle_gamma                105.798(3)
_cell_formula_units_Z            1
_cell_length_a                   20.5753(11)
_cell_length_b                   21.4339(13)
_cell_length_c                   27.9022(16)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.1
_cell_measurement_theta_min      2.20
_cell_volume                     10724.1(11)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.1025
_diffrn_reflns_av_unetI/netI     0.1296
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            108850
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        22.834
_diffrn_reflns_theta_max         22.834
_diffrn_reflns_theta_min         1.421
_diffrn_source                   '1uS Microfocus x-ray'
_exptl_absorpt_coefficient_mu    3.896
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.5997
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.237
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             6856
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.25
_refine_diff_density_min         -1.16
_refine_diff_density_rms         0.31
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1960
_refine_ls_number_reflns         28994
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1795
_refine_ls_R_factor_gt           0.0976
_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^)+(0.1485P)^2^+528.3792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2635
_refine_ls_wR_factor_ref         0.3280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15593
_reflns_number_total             28994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04398h2.cif
_cod_data_source_block           hz5336
_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               7120384
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.697
_shelx_estimated_absorpt_t_max   0.829
_shelx_res_checksum              63578