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_7133118
_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         'C33 H36 Br N'
_chemical_formula_sum            'C33 H36 Br N'
_chemical_formula_weight         526.54
_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             2023-01-19
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2024-03-20 deposited with the CCDC.	2024-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.3630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4197(3)
_cell_length_b                   14.0561(4)
_cell_length_c                   18.9616(6)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    153.00
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.18
_cell_volume                     2731.82(14)
_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      153.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest, PhotonIII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60778
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         1.987
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.526
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0910 before and 0.0414 after correction.
The Ratio of minimum to maximum transmission is 0.8849.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.879
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         6298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+2.7483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5491
_reflns_number_total             6298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02244k2.cif
_cod_data_source_block           sh_157n_0m
_cod_depositor_comments
'Adding full bibliography for 7133117--7133122.cif.'
_cod_database_code               7133118
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.595
_shelx_estimated_absorpt_t_min   0.547
_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.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C38(H38), C34(H34), C37(H37), C35(H35), C19(H19), C20(H20), C21(H21),
 C24(H24), C25(H25), C12(H12), C14(H14), C27(H27), C28(H28), C15(H15)
2.b Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C31(H31A,H31B,
 H31C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              20208
_shelx_hkl_checksum              89094
_olex2_submission_special_instructions 'No special instructions were received'