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_7719213
_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         'C52 H41 N5 P2 Zn'
_chemical_formula_sum            'C52 H41 N5 P2 Zn'
_chemical_formula_weight         863.21
_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   geom
_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                 92.0003(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.86347(8)
_cell_length_b                   20.78128(19)
_cell_length_c                   20.82638(17)
_cell_measurement_reflns_used    52248
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      80.0230
_cell_measurement_theta_min      2.9710
_cell_volume                     4266.30(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_sigmaI/netI    0.0816
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            106835
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.464
_diffrn_reflns_theta_min         3.005
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.839
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       prism
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.099
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         17417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0580
_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^)+(0.1186P)^2^+3.5544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1964
_refine_ls_wR_factor_ref         0.1996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16077
_reflns_number_total             17417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03402c2.cif
_cod_data_source_block           Compound4_Zn_KML090
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7719213
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.600
_shelx_estimated_absorpt_t_max   0.839
_shelx_res_checksum              43062
_shelx_hkl_checksum              32234