Cluster Synthesis via Ligand-Arrested Solid Growth: Triethylphosphine-Capped Fragments of Binary Metal Chalcogenides
Nathan R. M. Crawford; Allan G. Hee; Jeffrey R. Long; Journal of the American Chemical Society 124 (2002) 14842–14843; doi:10.1021/ja027862f

data_4115384
_publ_contact_author
;
        Jeffrey R. Long
        Department of Chemistry
        University of California, Berkeley
        United States of America
;
_publ_contact_author_email       jlong@cchem.berkeley.edu
_publ_contact_author_fax         '510 642-8369'
_publ_contact_author_phone       '510 642-0860'
_publ_section_title
;
 Cluster Synthesis via Ligand-Arrested Solid Growth:
 Triethylphosphine-Capped Fragments of Binary Metal Chalcogenides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14842
_journal_page_last               14843
_journal_paper_doi               10.1021/ja027862f
_journal_volume                  124
_journal_year                    2002
_chemical_compound_source        synthetic
_chemical_formula_structural     Cu70Se35(PEt3)21
_chemical_formula_sum            'C130 H325 Cu70 O P21 Se35'
_chemical_formula_weight         9766.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 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                 100.573(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.6986(15)
_cell_length_b                   35.504(3)
_cell_length_c                   29.214(2)
_cell_measurement_temperature    147(2)
_cell_volume                     26202(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      147(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       'CCD area detector'
_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  0.1692
_diffrn_reflns_av_sigmaI/netI    0.3304
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54020
_diffrn_reflns_theta_full        17.23
_diffrn_reflns_theta_max         17.23
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    10.561
_exptl_absorpt_correction_T_max  0.18
_exptl_absorpt_correction_T_min  0.02
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.476
_exptl_crystal_description       rod
_exptl_crystal_F_000             18592
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         5.229
_refine_diff_density_min         -2.983
_refine_diff_density_rms         0.577
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.56(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.313
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2111
_refine_ls_number_reflns         30349
_refine_ls_number_restraints     1655
_refine_ls_restrained_S_all      1.314
_refine_ls_R_factor_all          0.3223
_refine_ls_R_factor_gt           0.1581
_refine_ls_shift/su_max          0.333
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3400
_refine_ls_wR_factor_ref         0.4339
_reflns_number_gt                11339
_reflns_number_total             30349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja027862f_s2_1.cif
_cod_data_source_block           2
_cod_database_code               4115384