Mechanochemical and solution synthesis, and crystal structures and IR and solid-state (CPMAS) NMR spectroscopy of some bis(triphenylphosphine)silver(i) mono- and di-hydrogencitrate systems.
Bowmaker, Graham A.; Hanna, John V.; Skelton, Brian W.; White, Allan H.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 5409–5417; doi:10.1039/c2dt12452a

data_7018911
_publ_section_title
;
 Mechanochemical and solution synthesis, and crystal structures and IR and
 solid-state (CPMAS) NMR spectroscopy of some
 bis(triphenylphosphine)silver(i) mono- and di-hydrogencitrate systems.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5409
_journal_page_last               5417
_journal_paper_doi               10.1039/c2dt12452a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C78 H66 Ag2 O7 P4'
_chemical_formula_sum            'C78 H66 Ag2 O7 P4'
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_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-06-13T13:01:33-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.704(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.568(2)
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_cell_length_c                   23.1076(10)
_cell_measurement_reflns_used    5052
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.3915
_cell_measurement_theta_min      3.1061
_cell_volume                     6783.2(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_reduction
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type
;
Oxford Diffraction Gemini diffractometer
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_UB_11      0.0414916488
_diffrn_orient_matrix_UB_12      0.0313337205
_diffrn_orient_matrix_UB_13      0.0586292532
_diffrn_orient_matrix_UB_21      -0.0487008306
_diffrn_orient_matrix_UB_22      -0.0355018429
_diffrn_orient_matrix_UB_23      0.0272991076
_diffrn_orient_matrix_UB_31      0.0265998294
_diffrn_orient_matrix_UB_32      -0.1135970312
_diffrn_orient_matrix_UB_33      0.0076661876
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
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_exptl_absorpt_coefficient_mu    5.962
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;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         7.714
_refine_diff_density_min         -1.622
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         10450
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1776
_refine_ls_R_factor_gt           0.1271
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3289
_refine_ls_wR_factor_ref         0.3519
_reflns_number_gt                5353
_reflns_number_total             10450
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2dt12452a.txt
_cod_data_source_block           gban02
_cod_original_cell_volume        6783.2(7)
_cod_original_sg_symbol_Hall     -P_2ybc
_cod_database_code               7018911