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_7133122
_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
'C78 H98 Cl La N2 P2, 1.5(C4 H10 O), 0.4[C4H10O]'
_chemical_formula_sum            'C85.6 H117 Cl La N2 O1.9 P2'
_chemical_formula_weight         1440.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-09
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.01.24 svn.r2f8d729c for OlexSys, GUI svn.r6923)
;
_audit_update_record
;
2024-03-20 deposited with the CCDC.	2024-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.767(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.5986(13)
_cell_length_b                   24.7411(15)
_cell_length_c                   32.569(2)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      25.047
_cell_measurement_theta_min      2.201
_cell_volume                     16514.2(18)
_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 0.999
_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  0.1221
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            412057
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.923
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0960 before and 0.0578 after correction.
The Ratio of minimum to maximum transmission is 0.9042.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       block
_exptl_crystal_F_000             6110
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1738
_refine_ls_number_reflns         29081
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0415P)^2^+38.8695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22960
_reflns_number_total             29081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02244k2.cif
_cod_data_source_block           sh_405n_0m
_cod_depositor_comments
'Adding full bibliography for 7133117--7133122.cif.'
_cod_original_cell_volume        16514.1(19)
_cod_original_formula_sum        'C85.60 H117 Cl La N2 O1.90 P2'
_cod_database_code               7133122
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.800
_shelx_estimated_absorpt_t_min   0.764
_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
 C26A-C29A \\sim C26A-C29B
 with sigma of 0.02
 C29A-C32A \\sim C29B-C32B
 with sigma of 0.02
 C29A-C31A \\sim C29B-C31B
 with sigma of 0.02
 C29A-C30A \\sim C29B-C30B
 with sigma of 0.02
 C26A-C32A \\sim C26A-C32B
 with sigma of 0.04
 C26A-C31A \\sim C26A-C31B
 with sigma of 0.04
 C26A-C30A \\sim C26A-C30B
 with sigma of 0.04
 C32A-C31A \\sim C32B-C31B
 with sigma of 0.04
 C32A-C30A \\sim C32B-C30B
 with sigma of 0.04
 C31A-C30A \\sim C31B-C30B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C30B) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C31B) \\sim Ueq,
Uanis(C32A) \\sim Ueq, Uanis(C32B) \\sim Ueq, Uanis(C30A) \\sim Ueq,
Uanis(C29B) \\sim Ueq, Uanis(C29A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Sof(C29B)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31B)=Sof(H31D)=
 Sof(H31E)=Sof(H31F)=Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(1)
 Sof(C29A)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C31A)=Sof(H31A)=
 Sof(H31B)=Sof(H31C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C86A(H86A), C83A(H83A), C46A(H46A), C86(H86), C43A(H43A), C46(H46), C83(H83),
 C43(H43)
5.b Secondary CH2 refined with riding coordinates:
 C201(H20B,H20C), C301(H30J,H30K), C202(H20G,H20H), C102(H10D,H10E), C302(H30O,
 H30P), C101(H10I,H10J)
5.c Aromatic/amide H refined with riding coordinates:
 C55(H55), C21A(H21A), C60A(H60A), C74(H74), C61(H61), C78A(H78A), C59(H59),
 C60(H60), C77A(H77A), C55A(H55A), C68A(H68A), C61A(H61A), C59A(H59A),
 C38A(H38A), C15(H15), C64A(H64A), C64(H64), C19A(H19A), C65A(H65A), C28A(H28A),
  C67(H67), C77(H77), C75A(H75A), C20A(H20A), C78(H78), C68(H68), C34A(H34A),
 C75(H75), C54A(H54A), C54(H54), C35(H35), C34(H34), C27A(H27A), C74A(H74A),
 C15A(H15A), C38(H38), C12A(H12A), C21(H21), C52A(H52A), C14(H14), C67A(H67A),
 C35A(H35A), C12(H12), C25(H25), C37A(H37A), C19(H19), C24A(H24A), C14A(H14A),
 C25A(H25A), C52(H52), C37(H37), C65(H65), C27(H27), C28(H28), C20(H20),
 C24(H24)
5.d Idealised Me refined as rotating group:
 C82A(H82A,H82B,H82C), C87A(H87A,H87B,H87C), C84A(H84A,H84B,H84C), C88A(H88A,
 H88B,H88C), C48A(H48A,H48B,H48C), C88(H88D,H88E,H88F), C87(H87D,H87E,H87F),
 C85A(H85A,H85B,H85C), C56A(H56A,H56B,H56C), C44(H44D,H44E,H44F), C56(H56D,H56E,
 H56F), C48(H48D,H48E,H48F), C44A(H44A,H44B,H44C), C47A(H47A,H47B,H47C),
 C84(H84D,H84E,H84F), C45(H45D,H45E,H45F), C16A(H16A,H16B,H16C), C45A(H45A,H45B,
 H45C), C80A(H80A,H80B,H80C), C70(H70D,H70E,H70F), C82(H82D,H82E,H82F),
 C85(H85D,H85E,H85F), C81A(H81A,H81B,H81C), C47(H47D,H47E,H47F), C16(H16D,H16E,
 H16F), C32(H32G,H32H,H32I), C72(H72D,H72E,H72F), C30(H30G,H30H,H30I),
 C40A(H40A,H40B,H40C), C71(H71D,H71E,H71F), C80(H80D,H80E,H80F), C31(H31G,H31H,
 H31I), C72A(H72A,H72B,H72C), C41(H41D,H41E,H41F), C81(H81D,H81E,H81F),
 C71A(H71A,H71B,H71C), C41A(H41A,H41B,H41C), C42A(H42A,H42B,H42C), C70A(H70A,
 H70B,H70C), C42(H42D,H42E,H42F), C103(H10A,H10B,H10C), C40(H40D,H40E,H40F),
 C200(H20D,H20E,H20F), C32A(H32A,H32B,H32C), C31A(H31A,H31B,H31C), C100(H10F,
 H10G,H10H), C30A(H30A,H30B,H30C), C303(H30L,H30M,H30N), C300(H30Q,H30R,H30S),
 C203(H20I,H20J,H20K), C30B(H30D,H30E,H30F), C31B(H31D,H31E,H31F), C32B(H32D,
 H32E,H32F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 160 electrons were 
found in a volume of 2448\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
0.4[C4H10O] per Asymmetric Unit 
which account for 134 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              40712
_shelx_hkl_checksum              15403
_shelx_fab_checksum              95451
_olex2_submission_special_instructions 'No special instructions were received'