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_7127476
_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         'C62 H84 La N2 P4, C18 H36 K N2 O6'
_chemical_formula_sum            'C80 H120 K La N4 O6 P4'
_chemical_formula_weight         1535.68
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-14
_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                105.16(3)
_cell_angle_beta                 97.23(3)
_cell_angle_gamma                104.28(3)
_cell_formula_units_Z            2
_cell_length_a                   14.168(15)
_cell_length_b                   18.79(2)
_cell_length_c                   19.86(2)
_cell_measurement_reflns_used    6842
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.98
_cell_volume                     4842(9)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.3354
_diffrn_reflns_av_unetI/netI     0.3263
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53580
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.980
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1439 before and 0.1080 after correction.
The Ratio of minimum to maximum transmission is 0.6029.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.053
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.839
_refine_diff_density_min         -2.263
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         16395
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.2041
_refine_ls_R_factor_gt           0.0981
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0537P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2147
_refine_ls_wR_factor_ref         0.2883
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6842
_reflns_number_total             16395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06670b2.cif
_cod_data_source_block           sh_0069n_0m
_cod_depositor_comments
'Adding full bibliography for 7127476--7127479.cif.'
_cod_original_cell_volume        4841(9)
_cod_database_code               7127476
_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. Uiso/Uaniso restraints and constraints
Uanis(C303) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C26(H26), C59(H59), C29(H29), C56(H56)
3.b Secondary CH2 refined with riding coordinates:
 C302(H30D,H30E), C304(H30F,H30G), C300(H30H,H30I), C303(H30J,H30K), C105(H10A,
 H10B), C100(H10C,H10D), C104(H10E,H10F), C205(H20A,H20B), C200(H20C,H20D),
 C201(H20E,H20F), C101(H10G,H10H), C204(H20G,H20H), C103(H10I,H10J), C305(H30L,
 H30M), C203(H20I,H20J), C102(H10K,H10L), C301(H30N,H30O), C202(H20K,H20L)
3.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C15(H15), C14(H14), C12(H12), C51(H51), C19(H19), C72(H72),
 C82(H82), C42(H42), C84(H84), C45(H45), C49(H49), C44(H44), C74(H74)
3.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C55(H55A,H55B,H55C), C78(H78A,H78B,H78C), C28(H28A,H28B,
 H28C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C53(H53A,H53B,H53C), C86(H86A,
 H86B,H86C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C88(H88A,H88B,H88C),
 C61(H61A,H61B,H61C), C87(H87A,H87B,H87C), C76(H76A,H76B,H76C), C54(H54A,H54B,
 H54C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C58(H58A,H58B,H58C), C60(H60A,
 H60B,H60C), C77(H77A,H77B,H77C), C46(H46A,H46B,H46C), C57(H57A,H57B,H57C)
;
_olex2_submission_special_instructions 'No special instructions were received'