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_7019631
_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 H60 Ag2 Cl2 N4 P4, 2(C H4 O)'
_chemical_formula_sum            'C60 H68 Ag2 Cl2 N4 O2 P4'
_chemical_formula_weight         1287.70
_chemical_name_systematic
;
?
;
_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
_cell_angle_alpha                109.74(3)
_cell_angle_beta                 98.42(3)
_cell_angle_gamma                91.44(3)
_cell_formula_units_Z            1
_cell_length_a                   9.814(2)
_cell_length_b                   11.780(2)
_cell_length_c                   13.337(3)
_cell_measurement_reflns_used    6668
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.4971
_cell_measurement_theta_min      3.1682
_cell_volume                     1431.0(6)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13124
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.29
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7447
_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    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0398P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                5471
_reflns_number_total             6420
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30860f.txt
_cod_data_source_block           3^.^2CH^3^OH
_cod_original_cell_volume        1431.0(5)
_cod_database_code               7019631