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_1572113
_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         'C43 H62 N2 O P Y, C4 H8 O'
_chemical_formula_sum            'C47 H70 N2 O2 P Y'
_chemical_formula_weight         814.93
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_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                 99.158(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0823(13)
_cell_length_b                   28.934(4)
_cell_length_c                   15.635(2)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.16
_cell_volume                     4502.9(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0650
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38274
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.296
_diffrn_reflns_theta_min         2.164
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1510 before and 0.0700 after correction.
The Ratio of minimum to maximum transmission is 0.8412.
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    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         11171
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0526P)^2^+1.1172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8799
_reflns_number_total             11171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02077d2.cif
_cod_data_source_block           BiAmpYInd
_cod_depositor_comments
'Adding full bibliography for 1572109--1572117.cif.'
_cod_original_cell_volume        4503.1(10)
_cod_database_code               1572113
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.624
_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:
 C28(H28), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
 C43(H43A,H43B), C46(H46A,H46B), C45(H45A,H45B), C44(H44A,H44B), C47(H47A,H47B)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C36(H36), C35(H35), C20(H20), C18(H18), C16(H16), C12(H12),
 C10(H10), C8(H8)
2.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C22(H22A,H22B,H22C), C21(H21A,
 H21B,H21C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C14(H14A,H14B,
 H14C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              52117
_olex2_submission_special_instructions 'No special instructions were received'