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_7018912
_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         'C42 H37 Ag O7 P2, C2 H6 O'
_chemical_formula_sum            'C44 H43 Ag O8 P2'
_chemical_formula_weight         869.59
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-06-13T16:45:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                82.679(2)
_cell_angle_beta                 87.727(3)
_cell_angle_gamma                64.362(4)
_cell_formula_units_Z            2
_cell_length_a                   12.2314(5)
_cell_length_b                   12.8542(5)
_cell_length_c                   14.4510(4)
_cell_measurement_reflns_used    14089
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.2387
_cell_measurement_theta_min      2.8347
_cell_volume                     2031.36(15)
_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
;
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 16.0009
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.94
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_UB_11      0.0530216971
_diffrn_orient_matrix_UB_12      0.0095855383
_diffrn_orient_matrix_UB_13      -0.0025661248
_diffrn_orient_matrix_UB_21      -0.0289340583
_diffrn_orient_matrix_UB_22      0.0480990504
_diffrn_orient_matrix_UB_23      0.0256373012
_diffrn_orient_matrix_UB_31      0.0221035717
_diffrn_orient_matrix_UB_32      -0.0374424632
_diffrn_orient_matrix_UB_33      0.0422462281
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.099
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
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_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37387
_diffrn_reflns_theta_full        32.25
_diffrn_reflns_theta_max         33.35
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.99241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.155
_refine_diff_density_min         -0.58
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         14800
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                9552
_reflns_number_total             14800
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2dt12452a.txt
_cod_data_source_block           gban03
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               7018912