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_7129790
_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         '2(C35 H25 Yb0.5), 9(C3 H3)'
_chemical_formula_sum            'C97 H77 Yb'
_chemical_formula_weight         1415.62
_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
_audit_creation_date             2021-06-19
_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                83.15(3)
_cell_angle_beta                 87.83(3)
_cell_angle_gamma                79.75(3)
_cell_formula_units_Z            2
_cell_length_a                   12.870(3)
_cell_length_b                   13.490(3)
_cell_length_c                   21.010(4)
_cell_measurement_reflns_used    12701
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     3563.3(14)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            61483
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         0.976
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       block
_exptl_crystal_F_000             1458
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.754
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         12701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0548P)^2^+2.5079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11310
_reflns_number_total             12701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00698g2.cif
_cod_data_source_block           1_a
_cod_original_cell_volume        3563.4(13)
_cod_database_code               7129790
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.899
_exptl_absorpt_special_details   'not measured'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C66(H66), C35(H35), C13(H13), C42(H42), C7(H7), C17(H17), C31(H31),
 C25(H25), C63(H63), C64(H64), C19(H19), C60(H60), C29(H29), C14(H14), C70(H70),
  C26(H26), C22(H22), C11(H11), C21(H21), C52(H52), C58(H58), C61(H61),
 C15(H15), C69(H69), C20(H20), C34(H34), C48(H48), C46(H46), C56(H56), C57(H57),
  C62(H62), C28(H28), C54(H54), C27(H27), C33(H33), C51(H51), C9(H9), C49(H49),
 C32(H32), C96(H96), C67(H67), C8(H8), C50(H50), C16(H16), C95(H95), C45(H45),
 C55(H55), C43(H43), C97(H97), C10(H10), C44(H44), C68(H68), C79(H79), C78(H78),
  C77(H77), C82(H82), C81(H81), C80(H80), C73(H73), C75(H75), C74(H74),
 C72(H72), C85(H85), C76(H76), C71(H71), C84(H84), C83(H83), C88(H88), C93(H93),
  C86(H86), C90(H90), C87(H87), C89(H89), C94(H94), C92(H92), C91(H91)
2.b Fitted hexagon refined as free rotating group:
 C79(C78,C77,C82,C81,C80)
;
_shelx_res_checksum              37695
_olex2_submission_special_instructions 'No special instructions were received'