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_7133120
_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         'C47 H69 K N O2 P'
_chemical_formula_sum            'C47 H69 K N O2 P'
_chemical_formula_weight         750.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-31
_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                90
_cell_angle_beta                 97.3740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4630(4)
_cell_length_b                   16.2623(5)
_cell_length_c                   24.9920(10)
_cell_measurement_reflns_used    9654
_cell_measurement_temperature    152.00
_cell_measurement_theta_max      25.118
_cell_measurement_theta_min      2.765
_cell_volume                     4620.3(3)
_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      152.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0556
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            113957
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.091
_diffrn_reflns_theta_max         25.091
_diffrn_reflns_theta_min         2.186
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1459 before and 0.0726 after correction.
The Ratio of minimum to maximum transmission is 0.8570.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8187
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0703P)^2^+2.4759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7511
_reflns_number_total             8187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02244k2.cif
_cod_data_source_block           sh_163n_0m
_cod_depositor_comments
'Adding full bibliography for 7133117--7133122.cif.'
_cod_database_code               7133120
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.914
_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
 C202-C203
 1.54 with sigma of 0.01
 O200-C202 \\sim O200-C1
 with sigma of 0.02
 C203-C202 \\sim C2-C1
 with sigma of 0.02
 O200-C203 \\sim O200-C2
 with sigma of 0.04
3. Others
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C1)=Sof(H1A)=Sof(H1B)=1-FVAR(1)
 Sof(C203)=Sof(H20F)=Sof(H20G)=Sof(H20H)=Sof(C202)=Sof(H20I)=Sof(H20J)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C46(H46), C43(H43)
4.b Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C201(H20A,H20B), C102(H10F,H10G), C202(H20I,H20J), C1(H1A,H1B)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C12(H12), C24(H24), C33(H33), C31(H31), C30(H30),
 C25(H25), C28(H28), C27(H27), C34(H34), C21(H21), C19(H19), C20(H20)
4.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C38(H38A,H38B,H38C), C47(H47A,H47B,H47C), C36(H36A,H36B,
 H36C), C48(H48A,H48B,H48C), C37(H37A,H37B,H37C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C42(H42A,H42B,H42C), C41(H41A,H41B,H41C), C40(H40A,H40B,H40C),
 C103(H10C,H10D,H10E), C200(H20C,H20D,H20E), C100(H10H,H10I,H10J), C203(H20F,
 H20G,H20H), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              71358
_shelx_hkl_checksum              80977
_olex2_submission_special_instructions 'No special instructions were received'