Flexible interactions of the rare-earth elements Y, La, and Lu with phosphorus in metallacyclohexane rings.
Minko, Yury; Fetrow, Taylor V.; Sharma, Shikha; Cashman, Brenna K.; Tondreau, Aaron M.; Chemical science 15 (2024) 12138–12147; doi:10.1039/d4sc02077d

data_1572117
_publ_section_title
;
 Flexible interactions of the rare-earth elements Y, La, and Lu with
 phosphorus in metallacyclohexane rings.
;
_journal_issue                   30
_journal_name_full               'Chemical science'
_journal_page_first              12138
_journal_page_last               12147
_journal_paper_doi               10.1039/d4sc02077d
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '2(C43 H62 N2 O P Y), 1.5(C4 H10 O)'
_chemical_formula_sum            'C92 H139 N4 O3.5 P2 Y2'
_chemical_formula_weight         1596.82
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2021-09-27
_audit_creation_method
;
Olex2 1.2
(compiled Apr  3 2018 11:26:26 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2024-01-24 deposited with the CCDC.	2024-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                98.801(3)
_cell_angle_beta                 105.570(3)
_cell_angle_gamma                99.416(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7857(14)
_cell_length_b                   18.839(2)
_cell_length_c                   19.534(2)
_cell_measurement_reflns_used    9636
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      2.35
_cell_volume                     4374.4(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.996
_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       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            74818
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.284
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.406
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0471 before and 0.0391 after correction.
The Ratio of minimum to maximum transmission is 0.9035.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       block
_exptl_crystal_F_000             1710
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         21611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0287P)^2^+2.2988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19157
_reflns_number_total             21611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02077d2.cif
_cod_data_source_block           BiAMPYInd_Ether
_cod_depositor_comments
'Adding full bibliography for 1572109--1572117.cif.'
_cod_original_cell_volume        4374.2(9)
_cod_original_formula_sum        'C92 H139 N4 O3.50 P2 Y2'
_cod_database_code               1572117
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.817
_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. Others
 Sof(C89A)=Sof(H89C)=Sof(H89D)=Sof(C90A)=Sof(H90D)=Sof(H90E)=Sof(H90F)=1-FVAR(1)
 Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(H90C)=FVAR(1)
 Fixed Sof: C91(0.5) H91A(0.5) H91B(0.5) C91A(0.5) H91C(0.5) H91D(0.5)
 C92A(0.5) H92A(0.5) H92B(0.5) H92C(0.5) C92(0.5) H92D(0.5) H92E(0.5) H92F(0.5)
3.a Ternary CH refined with riding coordinates:
 C28(H28), C31(H31), C74(H74), C71(H71)
3.b Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C01L(H01A,H01B), C44(H44A,H44B), C1(H1A,H1B), C43(H43A,H43B),
 C40(H40A,H40B), C41(H41A,H41B), C86(H86A,H86B), C83(H83A,H83B), C85(H85A,H85B),
  C45(H45A,H45B), C84(H84A,H84B), C87(H87A,H87B), C91(H91A,H91B), C91A(H91C,
 H91D), C89(H89A,H89B), C89A(H89C,H89D)
3.c Aromatic/amide H refined with riding coordinates:
 C78(H78), C66(H66), C35(H35), C20(H20), C18(H18), C16(H16), C79(H79),
 C36(H36), C51(H51), C53(H53), C8(H8), C61(H61), C10(H10), C63(H63), C59(H59),
 C23(H23), C55(H55), C12(H12)
3.d Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C), C33(H33A,H33B,H33C), C38(H38A,H38B,H38C), C82(H82A,H82B,
 H82C), C21(H21A,H21B,H21C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C49(H49A,H49B,
 H49C), C47(H47A,H47B,H47C), C39(H39A,H39B,H39C), C22(H22A,H22B,H22C), C32(H32A,
 H32B,H32C), C57(H57A,H57B,H57C), C64(H64A,H64B,H64C), C4(H4A,H4B,H4C),
 C56(H56A,H56B,H56C), C30(H30A,H30B,H30C), C75(H75A,H75B,H75C), C48(H48A,H48B,
 H48C), C72(H72A,H72B,H72C), C81(H81A,H81B,H81C), C29(H29A,H29B,H29C), C65(H65A,
 H65B,H65C), C14(H14A,H14B,H14C), C76(H76A,H76B,H76C), C13(H13A,H13B,H13C),
 C88(H88A,H88B,H88C), C90(H90A,H90B,H90C), C92A(H92A,H92B,H92C), C92(H92D,H92E,
 H92F), C90A(H90D,H90E,H90F)
;
_shelx_res_checksum              33612
_olex2_submission_special_instructions 'No special instructions were received'