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_7127478
_publ_section_title
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 A transient lanthanum phosphinidene complex.
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_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         'C53 H73 La N2 P3, C18 H36 K N2 O6'
_chemical_formula_sum            'C71 H109 K La N4 O6 P3'
_chemical_formula_weight         1385.54
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-04
_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                105.285(2)
_cell_angle_beta                 94.133(3)
_cell_angle_gamma                109.532(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7500(8)
_cell_length_b                   15.9812(8)
_cell_length_c                   21.2031(14)
_cell_measurement_reflns_used    15847
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      1.98
_cell_volume                     3866.2(4)
_computing_cell_refinement       'Bruker Apex3 suite, 2019'
_computing_data_collection       'Bruker Apex3 suite, 2019'
_computing_data_reduction        'Bruker Apex3 suite, 2019'
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0709
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            266834
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.515
_diffrn_reflns_theta_min         1.980
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1541 before and 0.0612 after correction.
The Ratio of minimum to maximum transmission is 0.9210.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         17757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+3.1871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15847
_reflns_number_total             17757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06670b2.cif
_cod_data_source_block           sh_0059n_0m
_cod_depositor_comments
'Adding full bibliography for 7127476--7127479.cif.'
_cod_database_code               7127478
_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.a Ternary CH refined with riding coordinates:
 C26(H26), C59(H59), C56(H56), C29(H29)
2.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C105(H10A,H10B), C305(H30D,H30E), C205(H20A,H20B), C104(H10C,
 H10D), C204(H20C,H20D), C203(H20E,H20F), C302(H30F,H30G), C304(H30H,H30I),
 C102(H10E,H10F), C300(H30J,H30K), C301(H30L,H30M), C303(H30N,H30O), C202(H20G,
 H20H), C201(H20I,H20J), C101(H10G,H10H), C200(H20K,H20L), C103(H10I,H10J),
 C100(H10K,H10L)
2.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C44(H44), C42(H42), C19(H19), C51(H51), C15(H15), C12(H12),
 C45(H45), C49(H49), C14(H14), C74(H74), C72(H72)
2.d Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C24(H24A,H24B,
 H24C), C53(H53A,H53B,H53C), C28(H28A,H28B,H28C), C55(H55A,H55B,H55C), C30(H30A,
 H30B,H30C), C46(H46A,H46B,H46C), C60(H60A,H60B,H60C), C58(H58A,H58B,H58C),
 C31(H31A,H31B,H31C), C61(H61A,H61B,H61C), C54(H54A,H54B,H54C), C78(H78A,H78B,
 H78C), C76(H76A,H76B,H76C), C16(H16A,H16B,H16C), C77(H77A,H77B,H77C)
;
_olex2_submission_special_instructions 'No special instructions were received'

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