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_4115385
_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     Cu26Se13(PEt3)14
_chemical_formula_sum            'C84 H210 Cu26 P14 Se13'
_chemical_formula_weight         4332.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.305(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.2391(7)
_cell_length_b                   23.4906(10)
_cell_length_c                   17.3030(12)
_cell_measurement_temperature    130(2)
_cell_volume                     7006.9(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       '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  0.0781
_diffrn_reflns_av_sigmaI/netI    0.1140
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14276
_diffrn_reflns_theta_max         23.23
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    7.420
_exptl_absorpt_correction_T_max  0.44
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_description       block
_exptl_crystal_F_000             4240
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.483
_refine_diff_density_min         -1.382
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.078
_refine_ls_goodness_of_fit_obs   1.370
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5128
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.077
_refine_ls_restrained_S_obs      1.360
_refine_ls_R_factor_all          0.1757
_refine_ls_R_factor_obs          0.0925
_refine_ls_shift/esd_max         0.119
_refine_ls_shift/esd_mean        0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1279P)^2^+48.0972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2745
_refine_ls_wR_factor_obs         0.2391
_reflns_number_observed          2508
_reflns_number_total             5128
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja027862f_s2_2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1279P)^2^+48.0972P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1279P)^2^+48.0972P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4115385