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_7133121
_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         'C164 H216 Cl10 K2 La4 N4 O2 P4'
_chemical_formula_sum            'C164 H216 Cl10 K2 La4 N4 O2 P4'
_chemical_formula_weight         3387.61
_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             2024-03-01
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-20 deposited with the CCDC.	2024-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                98.117(3)
_cell_angle_beta                 100.137(3)
_cell_angle_gamma                108.631(4)
_cell_formula_units_Z            1
_cell_length_a                   12.8330(13)
_cell_length_b                   16.6810(17)
_cell_length_c                   21.1112(18)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      24.945
_cell_measurement_theta_min      2.316
_cell_volume                     4120.0(7)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.1310
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            179841
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.460
_diffrn_reflns_theta_min         2.189
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.318
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1272 before and 0.0864 after correction.
The Ratio of minimum to maximum transmission is 0.9179.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       plate
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     971
_refine_ls_number_reflns         16929
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+9.0941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13006
_reflns_number_total             16929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02244k2.cif
_cod_data_source_block           sh_423n_0m
_cod_depositor_comments
'Adding full bibliography for 7133117--7133122.cif.'
_cod_database_code               7133121
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.743
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P2-C86B \\sim P2-C86A
 with sigma of 0.02
 C86B-C87B \\sim C86A-C88A
 with sigma of 0.02
 C86B-C88B \\sim C86A-C87A
 with sigma of 0.02
 P2-C87B \\sim P2-C88A
 with sigma of 0.04
 P2-C86C \\sim P2-C86B \\sim P2-C86A
 with sigma of 0.02
 P2-C88B \\sim P2-C87A
 with sigma of 0.04
 C88C-C86C \\sim C88B-C86B \\sim C86A-C88A \\sim C87B-C86B \\sim C87A-C86A
\\sim C86C-C87C
 with sigma of 0.02
 C87B-C88B \\sim C88A-C87A
 with sigma of 0.04
 P2-C83B \\sim P2-C83A
 with sigma of 0.02
 C83B-C85B \\sim C83A-C85A
 with sigma of 0.02
 C83B-C84B \\sim C83A-C84A
 with sigma of 0.02
 P2-C85B \\sim P2-C85A
 with sigma of 0.04
 P2-C84B \\sim P2-C84A
 with sigma of 0.04
 C85B-C84B \\sim C85A-C84A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C88B \\sim C88A \\sim C87A \\sim C87B \\sim C86A \\sim C86B: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.02 within 1.7A
C86B \\sim C87B \\sim C88B \\sim C88A \\sim C86A \\sim C87A \\sim C87C \\sim
C86C \\sim C88C: within 1.9A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.9A
Uanis(C84A) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C85B) \\sim Ueq, Uanis(C83B)
\\sim Ueq, Uanis(C84B) \\sim Ueq, Uanis(C83A) \\sim Ueq, Uanis(C85A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 1*[Sof(C87C)+Sof(H87G)+Sof(H87H)+Sof(H87I)+Sof(C86C)+Sof(H86C)+Sof(C88C)+
 Sof(H88G)+Sof(H88H)+Sof(H88I)]+1*[Sof(C88A)+Sof(H88D)+Sof(H88E)+Sof(H88F)+
 Sof(C86A)+Sof(H86A)+Sof(C87A)+Sof(H87D)+Sof(H87E)+Sof(H87F)]+1*[Sof(C86B)+
 Sof(H86B)+Sof(C87B)+Sof(H87A)+Sof(H87B)+Sof(H87C)+Sof(C88B)+Sof(H88A)+
 Sof(H88B)+Sof(H88C)]=1 with esd of 0.0001
 Sof(C86B)=Sof(H86B)=Sof(C87B)=Sof(H87A)=Sof(H87B)=Sof(H87C)=Sof(C88B)=
 Sof(H88A)=Sof(H88B)=Sof(H88C)=FVAR(1)
 Sof(C85A)=Sof(H85D)=Sof(H85E)=Sof(H85F)=Sof(C83A)=Sof(H83A)=Sof(C84A)=
 Sof(H84D)=Sof(H84E)=Sof(H84F)=1-FVAR(2)
 Sof(C83B)=Sof(H83B)=Sof(C85B)=Sof(H85A)=Sof(H85B)=Sof(H85C)=Sof(C84B)=
 Sof(H84A)=Sof(H84B)=Sof(H84C)=FVAR(2)
 Sof(C87C)=Sof(H87G)=Sof(H87H)=Sof(H87I)=Sof(C86C)=Sof(H86C)=Sof(C88C)=
 Sof(H88G)=Sof(H88H)=Sof(H88I)=FVAR(3)
 Sof(C88A)=Sof(H88D)=Sof(H88E)=Sof(H88F)=Sof(C86A)=Sof(H86A)=Sof(C87A)=
 Sof(H87D)=Sof(H87E)=Sof(H87F)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C46(H46), C43(H43), C83B(H83B), C86B(H86B), C86A(H86A), C83A(H83A), C86C(H86C)
5.b Secondary CH2 refined with riding coordinates:
 C102(H10A,H10B), C101(H10C,H10D)
5.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C24(H24), C14(H14), C25(H25), C59(H59), C74(H74), C21(H21),
 C52(H52), C78(H78), C68(H68), C28(H28), C34(H34), C12(H12), C55(H55), C65(H65),
  C77(H77), C37(H37), C38(H38), C67(H67), C20(H20), C61(H61), C64(H64),
 C75(H75), C54(H54), C19(H19), C60(H60), C35(H35), C27(H27)
5.d Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C), C47(H47A,H47B,H47C), C16(H16A,H16B,H16C), C41(H41A,H41B,
 H41C), C48(H48A,H48B,H48C), C45(H45A,H45B,H45C), C42(H42A,H42B,H42C), C71(H71A,
 H71B,H71C), C40(H40A,H40B,H40C), C56(H56A,H56B,H56C), C30(H30A,H30B,H30C),
 C72(H72A,H72B,H72C), C44(H44A,H44B,H44C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C85B(H85A,H85B,H85C), C103(H10E,H10F,H10G), C80(H80A,H80B,H80C),
 C87B(H87A,H87B,H87C), C84B(H84A,H84B,H84C), C100(H10H,H10I,H10J), C81(H81A,
 H81B,H81C), C82(H82A,H82B,H82C), C88B(H88A,H88B,H88C), C88A(H88D,H88E,H88F),
 C87A(H87D,H87E,H87F), C85A(H85D,H85E,H85F), C84A(H84D,H84E,H84F), C87C(H87G,
 H87H,H87I), C88C(H88G,H88H,H88I)
;
_shelx_res_checksum              19052
_shelx_hkl_checksum              29044
_olex2_submission_special_instructions 'No special instructions were received'