Selective carbon-phosphorus bond cleavage: expanding the toolbox for accessing bulky divalent lanthanoid sandwich complexes
Shephard, Angus; Daniels, Daisy; Deacon, Glen B.; Guo, Zhifang; Jaroschik, Florian; Junk, Peter Courtney; Chemical Communications  (2022) –; doi:10.1039/D2CC00698G

data_7129788
_publ_section_title
;
 Selective carbon-phosphorus bond cleavage: expanding the toolbox for
 accessing bulky divalent lanthanoid sandwich complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00698G
_journal_year                    2022
_chemical_formula_moiety         'C74 H74 I2 O4 Yb2, 4(C6 H6)'
_chemical_formula_sum            'C98 H98 I2 O4 Yb2'
_chemical_formula_weight         1939.64
_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             2021-06-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-02-04 deposited with the CCDC.	2022-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                88.2270(10)
_cell_angle_beta                 80.3900(10)
_cell_angle_gamma                82.4170(10)
_cell_formula_units_Z            1
_cell_length_a                   11.9588(2)
_cell_length_b                   12.29030(10)
_cell_length_c                   14.33660(10)
_cell_measurement_reflns_used    23432
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      77.0740
_cell_measurement_theta_min      3.6330
_cell_volume                     2059.33(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41407
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.032
_diffrn_reflns_theta_min         3.628
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.367
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.505
_refine_diff_density_min         -1.332
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7811
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+2.9123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7313
_reflns_number_total             7811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00698g2.cif
_cod_data_source_block           1
_cod_database_code               7129788
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.424
_shelx_estimated_absorpt_t_min   0.231
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C42-C43
 1 with sigma of 0.02
3. Rigid bond restraints
 C38, C43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C42, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C41 \\sim C42: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2A
C43 \\sim C38: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2A
5.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C33(H33A,H33B), C34(H34A,H34B), C31(H31A,H31B), C32(H32A,
 H32B), C37(H37A,H37B), C35(H35A,H35B), C36(H36A,H36B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C25(H25), C17(H17), C23(H23), C15(H15), C29(H29), C13(H13), C20(H20),
 C8(H8), C14(H14), C11(H11), C16(H16), C21(H21), C19(H19), C26(H26), C22(H22),
 C7(H7), C9(H9), C28(H28), C27(H27), C10(H10), C38(H38), C46(H46), C47(H47),
 C48(H48), C45(H45), C42(H42), C41(H41), C49(H49), C39(H39), C43(H43), C44(H44),
  C40(H40)
;
_shelx_res_checksum              13603
_olex2_submission_special_instructions 'No special instructions were received'