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_7127477
_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         'C65 H96 K La N2 O7 P2'
_chemical_formula_sum            'C65 H96 K La N2 O7 P2'
_chemical_formula_weight         1257.38
_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             2020-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-01 deposited with the CCDC.	2020-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                116.117(2)
_cell_angle_beta                 98.326(2)
_cell_angle_gamma                99.911(2)
_cell_formula_units_Z            4
_cell_length_a                   13.3178(9)
_cell_length_b                   25.2864(17)
_cell_length_c                   25.5213(17)
_cell_measurement_reflns_used    24047
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      2.036
_cell_measurement_theta_min      27.096
_cell_volume                     7361.7(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 0.999
_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  0.0938
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            672658
_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         27.096
_diffrn_reflns_theta_min         2.036
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1284 before and 0.0567 after correction.
The Ratio of minimum to maximum transmission is 0.8833.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.627
_refine_diff_density_min         -1.625
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1441
_refine_ls_number_reflns         32352
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0440P)^2^+27.7958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1437
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24047
_reflns_number_total             32352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06670b2.cif
_cod_data_source_block           fw_0124n_0m
_cod_depositor_comments
;
Adding full bibliography for 7127476--7127479.cif.

2024-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C130 H192 K2 La2 N4 O14 P4'
_cod_original_formula_weight         2514.76
_cod_original_formula_moiety         '2(C65 H96 K La N2 O7 P2)'
_cod_original_formula_units_Z            2
_cod_database_code               7127477
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.834
_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(C56A) \\sim Ueq, Uanis(C57A) \\sim Ueq, Uanis(C58A) \\sim Ueq,
Uanis(C59A) \\sim Ueq, Uanis(C60A) \\sim Ueq, Uanis(C61A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C29(H29), C56(H56), C59(H59), C26(H26), C29A(H29A), C26A(H26A), C56A(H56A),
 C59A(H59A)
3.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C111(H11A,H11B), C110(H11C,H11D), C104(H10A,H10B), C103(H10C,
 H10D), C101(H10E,H10F), C25A(H25C,H25D), C105(H10G,H10H), C102(H10I,H10J),
 C100(H10K,H10L), C108(H10M,H10N), C109(H10O,H10P), C106(H10Q,H10R), C107(H10S,
 H10T), C206(H20A,H20B), C209(H20C,H20D), C201(H20E,H20F), C210(H21B,H21C),
 C205(H20G,H20H), C204(H20I,H20J), C200(H20K,H20L), C208(H20M,H20N), C207(H20O,
 H20P), C202(H20Q,H20R), C203(H20S,H20T), C211(H21D,H21E)
3.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C15(H15), C19A(H19A), C14(H14), C42(H42), C12(H12), C72A(H72A),
 C44A(H44A), C19(H19), C45A(H45A), C21A(H21A), C42A(H42A), C51A(H51A), C45(H45),
  C12A(H12A), C15A(H15A), C44(H44), C14A(H14A), C49(H49), C74A(H74A), C51(H51),
 C49A(H49A), C74(H74), C72(H72)
3.d Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C23(H23A,H23B,H23C), C60(H60A,H60B,H60C), C53(H53A,H53B,
 H53C), C61(H61A,H61B,H61C), C77A(H77D,H77E,H77F), C23A(H23D,H23E,H23F),
 C27(H27A,H27B,H27C), C76A(H76D,H76E,H76F), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C55A(H55D,H55E,H55F), C76(H76A,H76B,H76C), C28(H28A,H28B,H28C),
 C57(H57A,H57B,H57C), C16(H16A,H16B,H16C), C46A(H46D,H46E,H46F), C27A(H27D,H27E,
 H27F), C46(H46A,H46B,H46C), C55(H55A,H55B,H55C), C24(H24A,H24B,H24C),
 C53A(H53D,H53E,H53F), C78(H78A,H78B,H78C), C24A(H24D,H24E,H24F), C31A(H31D,
 H31E,H31F), C78A(H78D,H78E,H78F), C30A(H30D,H30E,H30F), C54(H54A,H54B,H54C),
 C16A(H16D,H16E,H16F), C54A(H54D,H54E,H54F), C28A(H28D,H28E,H28F), C77(H77A,
 H77B,H77C), C61A(H61D,H61E,H61F), C57A(H57D,H57E,H57F), C60A(H60D,H60E,H60F),
 C58A(H58D,H58E,H58F)
;