Formation of N-heterocyclic diphosphine ligands from Ag(i)-assisted condensation reactions between bdppeda and formaldehyde and their binuclear silver(i) complexes.
Sun, Sha; Ren, Zhi-Gang; Yang, Ju-Hua; He, Run-Tian; Wang, Fan; Wu, Xin-Yi; Gong, Wei-Jie; Li, Hong-Xi; Lang, Jian-Ping; Dalton transactions (Cambridge, England : 2003) 41 (2012) 8447–8454; doi:10.1039/c2dt30860f

data_7019630
_publ_section_title
;
 Formation of N-heterocyclic diphosphine ligands from Ag(i)-assisted
 condensation reactions between bdppeda and formaldehyde and their
 binuclear silver(i) complexes.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8447
_journal_page_last               8454
_journal_paper_doi               10.1039/c2dt30860f
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety
'C58 H58 Ag2 Cl2 N4 P4, 2(Cl O4), 2(C H2 Cl2), 2(H2 O)'
_chemical_formula_sum            'C60 H66 Ag2 Cl8 N4 O10 P4'
_chemical_formula_weight         1626.39
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.03(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.601(3)
_cell_length_b                   14.615(3)
_cell_length_c                   17.145(3)
_cell_measurement_reflns_used    15087
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5049
_cell_measurement_theta_min      3.0301
_cell_volume                     3408.1(12)
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction
'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       /w
_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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30416
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.040
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.896
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.218
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+7.2445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1569
_reflns_number_gt                6913
_reflns_number_total             7801
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30860f.txt
_cod_data_source_block           2^.^2CH~2~Cl~2~^.^2H~2~O
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7019630