A new class of ligand derived from the reactions of bis(dialkylphosphino)amines and 9-diazofluorene: preparation, structure and reactivity.
Laprade, Matthew J. J.; Robertson, Katherine N.; Clyburne, Jason A. C.; Kozak, Christopher M.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11382–11397; doi:10.1039/d4dt03402c

data_7719211
_publ_section_title
;
 A new class of ligand derived from the reactions of
 bis(dialkylphosphino)amines and 9-diazofluorene: preparation, structure
 and reactivity.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11382
_journal_page_last               11397
_journal_paper_doi               10.1039/d4dt03402c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C50 H38 N5 P2, Cl, 2(C2 H3 N)'
_chemical_formula_sum            'C54 H44 Cl N7 P2'
_chemical_formula_weight         888.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-05-03 deposited with the CCDC.	2025-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.5420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.166(3)
_cell_length_b                   9.0650(10)
_cell_length_c                   20.185(2)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      28.83
_cell_measurement_theta_min      2.39
_cell_volume                     4581.6(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27173
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.951
_diffrn_reflns_theta_min         1.627
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker 2009'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.475
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         5740
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+3.8735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4748
_reflns_number_total             5740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03402c2.cif
_cod_data_source_block           Compound2b_CMJL020
_cod_original_cell_volume        4581.6(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7719211
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.911
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              27777
_shelx_hkl_checksum              18901