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_7133119
_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         'C105 H133 La2 N2 P5, C4 H10 O'
_chemical_formula_sum            'C109 H143 La2 N2 O P5'
_chemical_formula_weight         1929.92
_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   mixed
_audit_creation_date             2023-02-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-03-20 deposited with the CCDC.	2024-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                76.309(6)
_cell_angle_beta                 70.924(6)
_cell_angle_gamma                69.957(7)
_cell_formula_units_Z            2
_cell_length_a                   15.498(3)
_cell_length_b                   16.566(4)
_cell_length_c                   22.288(4)
_cell_measurement_reflns_used    9815
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      26.056
_cell_measurement_theta_min      2.196
_cell_volume                     5030.1(18)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker Apex 4 v2021.4-0'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.00
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON III C14'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'multi layered optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_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            147923
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.956
_diffrn_source                   'Incoatec Microfocus'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  0.9143
_exptl_absorpt_correction_T_min  0.8467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0812 before and 0.0632 after correction.
The Ratio of minimum to maximum transmission is 0.9261.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.204
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         18703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+4.1784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14825
_reflns_number_total             18703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02244k2.cif
_cod_data_source_block           sh170n
_cod_depositor_comments
'Adding full bibliography for 7133117--7133122.cif.'
_cod_original_cell_volume        5030.0(19)
_cod_database_code               7133119
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.885
_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.a Ternary CH refined with riding coordinates:
 C34(H34), C37(H37), C73(H73), C76(H76)
2.b Secondary CH2 refined with riding coordinates:
 C106(H10J,H10K), C108(H10O,H10P)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C18(H18), C19(H19), C25(H25), C26(H26), C28(H28), C29(H29), C42(H42), C44(H44),
  C45(H45), C49(H49), C50(H50), C51(H51), C54(H54), C55(H55), C57(H57),
 C58(H58), C64(H64), C65(H65), C67(H67), C68(H68), C81(H81), C83(H83), C90(H90),
  C92(H92), C99(H99), C101(H101)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C46(H46A,H46B,H46C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,
 H62C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C74(H74A,
 H74B,H74C), C75(H75A,H75B,H75C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C),
 C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C94(H94A,H94B,
 H94C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C103(H10A,H10B,H10C),
 C104(H10D,H10E,H10F), C105(H10G,H10H,H10I), C107(H10L,H10M,H10N), C109(H10Q,
 H10R,H10S)
;
_shelx_res_checksum              78119
_shelx_hkl_checksum              47088
_olex2_submission_special_instructions 'No special instructions were received'