Synthesis and structural characterization of inverse-coordination clusters from a two-electron superatomic copper nanocluster.
Chakrahari, Kiran Kumarvarma; Silalahi, Rhone P Brocha; Liao, Jian-Hong; Kahlal, Samia; Liu, Yu-Chiao; Lee, Jyh-Fu; Chiang, Ming-Hsi; Saillard, Jean-Yves; Liu, C. W.; Chemical science 9 (2018) 6785–6795; doi:10.1039/c8sc01508b

data_1549654
_publ_section_title
;
 Synthesis and structural characterization of inverse-coordination
 clusters from a two-electron superatomic copper nanocluster.
;
_journal_issue                   33
_journal_name_full               'Chemical science'
_journal_page_first              6785
_journal_page_last               6795
_journal_paper_doi               10.1039/c8sc01508b
_journal_volume                  9
_journal_year                    2018
_chemical_formula_sum            'C74 H128 Cu12 N6 O8 S13'
_chemical_formula_weight         2409.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1yy2xw
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-06-21 deposited with the CCDC.
2018-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1023(9)
_cell_length_b                   23.8001(11)
_cell_length_c                   24.5421(12)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.18
_cell_volume                     11157.7(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            125549
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.351
_exptl_absorpt_coefficient_mu    2.523
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       prism
_exptl_crystal_F_000             4936
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 6299 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1020
_refine_ls_number_reflns         19663
_refine_ls_number_restraints     581
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0490
_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^)+(0.1068P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1500
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                15675
_reflns_number_total             19663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01508b2.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 1549648--1549654.cif.'
_cod_database_code               1549654
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.371
_shelx_estimated_absorpt_t_max   0.769
_shelx_res_checksum              64545