A bridging bis-phosphanido-phosphinidene complex of lanthanum supported by a sterically encumbering PN ligand.
Wittwer, B.; Heim, F.; Wurst, K.; Hohloch, S.; Chemical communications (Cambridge, England) 60 (2024) 7299–7302; doi:10.1039/d4cc02244k

data_7133117
_publ_section_title
;
 A bridging bis-phosphanido-phosphinidene complex of lanthanum supported
 by a sterically encumbering PN ligand.
;
_journal_issue                   57
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7299
_journal_page_last               7302
_journal_paper_doi               10.1039/d4cc02244k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C39 H50 N P'
_chemical_formula_sum            'C39 H50 N P'
_chemical_formula_weight         563.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-24
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.01.27 svn.rdd5efbe3 for OlexSys, GUI svn.r6708)
;
_audit_update_record
;
2024-03-20 deposited with the CCDC.	2024-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                115.435(4)
_cell_angle_beta                 107.508(4)
_cell_angle_gamma                96.665(5)
_cell_formula_units_Z            2
_cell_length_a                   10.7562(12)
_cell_length_b                   13.4826(16)
_cell_length_c                   14.1323(17)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    153.00
_cell_measurement_theta_max      26.430
_cell_measurement_theta_min      2.297
_cell_volume                     1692.0(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      153.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 Quest, Photon III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32936
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.492
_diffrn_reflns_theta_min         2.118
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1134 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.7988.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description       block
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6950
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0564P)^2^+1.0131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5734
_reflns_number_total             6950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02244k2.cif
_cod_data_source_block           sh_0173n_0m
_cod_depositor_comments
'Adding full bibliography for 7133117--7133122.cif.'
_cod_original_cell_volume        1692.0(3)
_cod_database_code               7133117
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.963
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C35-C36A \\sim C35-C36
 with sigma of 0.02
 C35-C38A \\sim C35-C38
 with sigma of 0.02
 C35-C37A \\sim C35-C37
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C38A) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
4. Others
 Sof(C38)=Sof(H38d)=Sof(H38e)=Sof(H38f)=Sof(C36)=Sof(H36d)=Sof(H36e)=Sof(H36f)=
 Sof(C37)=Sof(H37d)=Sof(H37e)=Sof(H37f)=1-FVAR(1)
 Sof(C36A)=Sof(H36a)=Sof(H36b)=Sof(H36c)=Sof(C38A)=Sof(H38a)=Sof(H38b)=
 Sof(H38c)=Sof(C37A)=Sof(H37a)=Sof(H37b)=Sof(H37c)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C46(H46), C43(H43)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C15(H15), C12(H12), C28(H28), C14(H14), C27(H27), C33(H33), C31(H31),
 C30(H30), C34(H34), C21(H21), C24(H24), C20(H20), C19(H19), C25(H25)
5.c Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C44(H44a,H44b,H44c), C47(H47a,H47b,H47c), C48(H48a,H48b,
 H48c), C42(H42a,H42b,H42c), C45(H45a,H45b,H45c), C40(H40a,H40b,H40c), C41(H41a,
 H41b,H41c), C36A(H36a,H36b,H36c), C38A(H38a,H38b,H38c), C37A(H37a,H37b,H37c),
 C38(H38d,H38e,H38f), C36(H36d,H36e,H36f), C37(H37d,H37e,H37f)
;
_shelx_res_checksum              41601
_shelx_hkl_checksum              91012
_olex2_submission_special_instructions 'No special instructions were received'