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_7719212
_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_absolute_configuration ad
_chemical_formula_moiety         'C38 H46 N5 P2, Cl'
_chemical_formula_sum            'C38 H46 Cl N5 P2'
_chemical_formula_weight         670.19
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   44.675(8)
_cell_length_b                   12.046(2)
_cell_length_c                   13.484(2)
_cell_measurement_reflns_used    5127
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      24.39
_cell_measurement_theta_min      2.31
_cell_volume                     7256(2)
_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 0.998
_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  0.0936
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20166
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.151
_diffrn_reflns_theta_min         1.823
_exptl_absorpt_coefficient_mu    0.227
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker 2009'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       block
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.175
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 1116 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4020
_refine_ls_number_restraints     369
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0145P)^2^+14.6250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                3032
_reflns_number_total             4020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03402c2.cif
_cod_data_source_block           Compound2a_CMJL018
_cod_database_code               7719212
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.935
_shelx_estimated_absorpt_t_max   0.961
_shelx_res_checksum              1040
_shelx_hkl_checksum              24734