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_1572115
_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         'C47 H69 La N2 O2 P, 5.333(C0.75)'
_chemical_formula_sum            'C51 H69 La N2 O2 P'
_chemical_formula_weight         911.96
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-01-24
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2024-01-24 deposited with the CCDC.	2024-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.1393(6)
_cell_length_b                   21.1393(6)
_cell_length_c                   10.8270(4)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.15
_cell_volume                     4838.3(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_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  0.0804
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            87253
_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         28.329
_diffrn_reflns_theta_min         2.113
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1791 before and 0.0754 after correction.
The Ratio of minimum to maximum transmission is 0.8977.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6246
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0593P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0880
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5801
_reflns_number_total             6246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02077d2.cif
_cod_data_source_block           labiampind_thf
_cod_depositor_comments
'Adding full bibliography for 1572109--1572117.cif.'
_cod_database_code               1572115
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.818
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.98(2)
 0.02(2)
2. 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
3. Restrained distances
 C35-C36
 1.54 with sigma of 0.02
 C31-C32
 1.54 with sigma of 0.02
 C31-C30
 1.54 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
5. Others
 Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(C17A)=Sof(H17C)=Sof(H17D)=1-FVAR(1)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18C)=Sof(H18D)=FVAR(1)
 Fixed Sof: C16(0.5) H16A(0.5) H16B(0.5) H13A(0.5) H13B(0.5) H14A(0.5)
 H14B(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C15(0.5) H15A(0.5) H15B(0.5) C36(0.0625)
 C29(0.5) C35(0.125) C28(0.5) C30(0.25) C31(0.25) C32(0.125) C34(0.125)
 C33(0.0625)
6.a Ternary CH refined with riding coordinates:
 C25(H25)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C16(H16A,H16B), C13(H13A,H13B), C14(H14A,H14B), C17(H17A,H17B),
 C18A(H18A,H18B), C18(H18C,H18D), C17A(H17C,H17D), C15(H15A,H15B)
6.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C6(H6), C8(H8), C23(H23)
6.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C26(H26A,H26B,H26C), C12(H12A,H12B,H12C), C24(H24A,H24B,
 H24C), C4(H4A,H4B,H4C), C11(H11A,H11B,H11C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              64655
_olex2_exptl_crystal_mounting_method 'Krytox on a nylon loop.'
_olex2_submission_special_instructions 'No special instructions were received'