Comproportionation Synthesis of Copper(I) Alkynyl Complexes Encapsulating Polyoxomolybdate Templates: Bowl-Shaped Cu33 and Peanut-Shaped Cu62 Nanoclusters.
Zhang, Li-Min; Mak, Thomas C. W.; Journal of the American Chemical Society 138 (2016) 2909–2912; doi:10.1021/jacs.5b12103

data_4129948
_publ_section_title
;
 Comproportionation Synthesis of Copper(I) Alkynyl Complexes Encapsulating
 Polyoxomolybdate Templates: Bowl-Shaped Cu33 and Peanut-Shaped Cu62
 Nanoclusters.
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2909
_journal_page_last               2912
_journal_paper_doi               10.1021/jacs.5b12103
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C194 H288 B2 Cu34 F8 O2'
_chemical_formula_weight         4986.58
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.963(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.473(4)
_cell_length_b                   15.889(2)
_cell_length_c                   54.655(7)
_cell_measurement_reflns_used    9801
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.8
_cell_measurement_theta_min      2.3
_cell_volume                     22490(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            150346
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.76
_exptl_absorpt_coefficient_mu    3.184
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10144.0
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.181
_refine_diff_density_min         -1.926
_refine_diff_density_rms         0.415
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2303
_refine_ls_number_reflns         38158
_refine_ls_number_restraints     463
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1688
_refine_ls_R_factor_gt           0.1079
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1434P)^2^+352.0354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2745
_refine_ls_wR_factor_ref         0.3302
_reflns_number_gt                22874
_reflns_number_total             38158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b12103_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4129948