Crystal structures and vibrational and solid-state (CPMAS) NMR spectroscopic studies in the tris(triphenylphosphine)-copper(I) and -silver(I) formate systems
Bowmaker, Graham A.; Hanna, John V.; Healy, Peter C.; Reid, Jason C.; Rickard, Clifton E. F.; White, Allan H.; Journal of the Chemical Society, Dalton Transactions  (2000) 753–; doi:10.1039/a908427d

data_7009071
_publ_section_title
;
 Crystal structures and vibrational and solid-state (CPMAS) NMR
 spectroscopic studies in the tris(triphenylphosphine)-copper(I) and
 -silver(I) formate systems
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              753
_journal_paper_doi               10.1039/a908427d
_journal_year                    2000
_chemical_formula_moiety         'C55 H46 Cu O2 P3, 0.5(C2 H6 O)'
_chemical_formula_sum            'C56 H49 Cu O2.5 P3'
_chemical_formula_weight         918.40
_chemical_name_systematic
; 
 [Cu(PPh3)3O2CH].0.5EtOH
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_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                90.0000(10)
_cell_angle_beta                 93.57
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6750(10)
_cell_length_b                   22.4545(10)
_cell_length_c                   13.935
_cell_measurement_temperature    293(2)
_cell_volume                     4895.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     0.70173
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11651
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_T_max  0.8919
_exptl_absorpt_correction_T_min  0.7584
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1916
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         11651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.739
_refine_ls_shift/su_mean         0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1266P)^2^+4.3775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2159
_refine_ls_wR_factor_ref         0.2394
_reflns_number_gt                8871
_reflns_number_total             11651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a908427d.txt
_cod_data_source_block           a2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1266P)^2^+4.3775P] 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^)+(0.1266P)^2^+4.3775P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C56 H49 Cu O2.50 P3'
_cod_database_code               7009071