A new amido-phosphane as ligand for copper and silver complexes. Synthesis, characterization and catalytic application for azide-alkyne cycloaddition in glycerol.
Mahmoud, Abdallah G.; Guedes da Silva, M Fátima C; Pombeiro, Armando J. L.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6109–6125; doi:10.1039/d1dt00992c

data_7707089
_publ_section_title
;
 A new amido-phosphane as ligand for copper and silver complexes.
 Synthesis, characterization and catalytic application for azide-alkyne
 cycloaddition in glycerol.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6109
_journal_page_last               6125
_journal_paper_doi               10.1039/d1dt00992c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '2(C19 H20 N3 O2 P), H2 O'
_chemical_formula_sum            'C38 H42 N6 O5 P2'
_chemical_formula_weight         724.71
_chemical_name_systematic
1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane-3,7-diylbis(phenylmethanone)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-03-01 deposited with the CCDC.	2021-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.955(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5691(5)
_cell_length_b                   21.4898(12)
_cell_length_c                   10.0298(5)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.64
_cell_measurement_theta_min      2.39
_cell_volume                     1838.44(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SIR-2014 (Burla, 2015)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26254
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.106
_diffrn_reflns_theta_min         2.467
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             764
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone'
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.08(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         4024
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.1528
_refine_ls_R_factor_gt           0.1226
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1959P)^2^+2.3112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3516
_refine_ls_wR_factor_ref         0.3842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2779
_reflns_number_total             4024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00992c2.cif
_cod_data_source_block           DBPTA
_cod_depositor_comments          'Adding full bibliography for 7707089.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7707089
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.982
_shelx_res_checksum              7959
_shelx_hkl_checksum              89492