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_1572112
_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         'C34 H55 I Lu N2 O3 P'
_chemical_formula_sum            'C34 H55 I Lu N2 O3 P'
_chemical_formula_weight         872.64
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-03
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4115(9)
_cell_length_b                   14.1878(10)
_cell_length_c                   19.0912(14)
_cell_measurement_reflns_used    9823
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.35
_cell_volume                     3632.7(4)
_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 0.996
_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  0.0318
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35210
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.335
_diffrn_reflns_theta_min         3.063
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.645
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0661 before and 0.0516 after correction.
The Ratio of minimum to maximum transmission is 0.8078.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       plate
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.290(6)
_refine_ls_extinction_coef       0.00021(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         9000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0215
_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^)+4.4545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0443
_refine_ls_wR_factor_ref         0.0447
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                8672
_reflns_number_total             9000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02077d2.cif
_cod_data_source_block           2ndintlui
_cod_depositor_comments
'Adding full bibliography for 1572109--1572117.cif.'
_cod_database_code               1572112
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.501
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.710(6)
 0.290(6)
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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C29(H29A,H29B), C32(H32A,H32B), C28(H28A,H28B),
 C30(H30A,H30B), C25(H25A,H25B), C24(H24A,H24B), C31(H31A,H31B), C27(H27A,H27B),
  C21(H21A,H21B), C26(H26A,H26B), C23(H23A,H23B), C22(H22A,H22B)
3.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C12(H12), C8(H8), C16(H16), C18(H18), C10(H10)
3.c Idealised Me refined as rotating group:
 C00M(H00A,H00B,H00C), C14(H14A,H14B,H14C), C6(H6A,H6B,H6C), C13(H13A,H13B,
 H13C), C4(H4A,H4B,H4C), C012(H01A,H01B,H01C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              11993
_olex2_submission_special_instructions 'No special instructions were received'