A transient lanthanum phosphinidene complex.
Watt, Fabian A.; McCabe, Karl N.; Schoch, Roland; Maron, Laurent; Hohloch, Stephan; Chemical communications (Cambridge, England) 56 (2020) 15410–15413; doi:10.1039/d0cc06670b

data_7127479
_publ_section_title
;
 A transient lanthanum phosphinidene complex.
;
_journal_issue                   98
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              15410
_journal_page_last               15413
_journal_paper_doi               10.1039/d0cc06670b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '2(C65 H97 K La N2 O6 P3), C4 H10 O'
_chemical_formula_sum            'C134 H204 K2 La2 N4 O13 P6'
_chemical_formula_weight         2620.84
_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             2020-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-30 deposited with the CCDC.	2020-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                99.417(2)
_cell_angle_beta                 90.617(2)
_cell_angle_gamma                91.294(2)
_cell_formula_units_Z            1
_cell_length_a                   14.0506(8)
_cell_length_b                   14.3744(8)
_cell_length_c                   18.1614(10)
_cell_measurement_reflns_used    14757
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      1.97
_cell_volume                     3617.3(4)
_computing_cell_refinement       'Bruker Apex3 suite, 2020'
_computing_data_collection       'Bruker Apex3 suite, 2020'
_computing_data_reduction        'Bruker Apex3 suite, 2020'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'omega phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            337081
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.363
_diffrn_reflns_theta_min         1.973
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1364 before and 0.0528 after correction.
The Ratio of minimum to maximum transmission is 0.9018.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       block
_exptl_crystal_F_000             1382
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.842
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         14757
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+5.9270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13249
_reflns_number_total             14757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06670b2.cif
_cod_data_source_block           p
_cod_depositor_comments
'Adding full bibliography for 7127476--7127479.cif.'
_cod_database_code               7127479
_shelx_shelxl_version_number     2017/1
_exptl_absorpt_special_details   'Blessing, 1995'
_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
 C200-C201
 1.54 with sigma of 0.02
 C201-O200
 1.54 with sigma of 0.02
 O200-C202
 1.54 with sigma of 0.02
 C202-C203
 1.54 with sigma of 0.02
 H70-P70
 1.3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C200) \\sim Ueq, Uanis(C201) \\sim Ueq, Uanis(C202) \\sim Ueq,
Uanis(C203) \\sim Ueq, Uanis(O200) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: O200(0.5) C201(0.5) H20A(0.5) H20B(0.5) C203(0.5) H20C(0.5)
 H20D(0.5) H20E(0.5) C202(0.5) H20F(0.5) H20G(0.5) C200(0.5) H20H(0.5)
 H20I(0.5) H20J(0.5)
5.a Ternary CH refined with riding coordinates:
 C26(H26), C29(H29), C56(H56), C59(H59)
5.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C108(H10A,H10B), C107(H10C,H10D), C109(H10E,H10F), C106(H10G,
 H10H), C104(H10I,H10J), C111(H11A,H11B), C100(H10K,H10L), C105(H10M,H10N),
 C110(H11C,H11D), C101(H10O,H10P), C102(H10Q,H10R), C103(H10S,H10T), C201(H20A,
 H20B), C202(H20F,H20G)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C19(H19), C21(H21), C12(H12), C42(H42), C45(H45),
 C51(H51), C49(H49), C44(H44), C74(H74), C72(H72)
5.d Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C30(H30A,H30B,
 H30C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C16(H16A,H16B,H16C), C53(H53A,
 H53B,H53C), C27(H27A,H27B,H27C), C58(H58A,H58B,H58C), C61(H61A,H61B,H61C),
 C46(H46A,H46B,H46C), C57(H57A,H57B,H57C), C60(H60A,H60B,H60C), C78(H78A,H78B,
 H78C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C203(H20C,H20D,H20E),
 C200(H20H,H20I,H20J), C54(H54A,H54B,H54C)
;
_olex2_submission_special_instructions 'No special instructions were received'