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_7129789
_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         'C47 H35 P'
_chemical_formula_sum            'C47 H35 P'
_chemical_formula_weight         630.72
_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             2021-04-12
_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                96.14(3)
_cell_angle_beta                 90.06(3)
_cell_angle_gamma                115.02(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1150(18)
_cell_length_b                   10.483(2)
_cell_length_c                   19.585(4)
_cell_measurement_reflns_used    6286
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     1683.8(7)
_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 0.992
_diffrn_measured_fraction_theta_max 0.984
_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  0.0473
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49067
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_min         1.047
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.7
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0779P)^2^+0.4191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1224
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5945
_reflns_number_total             6286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00698g2.cif
_cod_data_source_block           merge
_cod_database_code               7129789
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.991
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C29(H29), C13(H13), C23(H23), C25(H25), C47(H47), C35(H35), C17(H17),
 C31(H31), C19(H19), C22(H22), C11(H11), C37(H37), C10(H10), C32(H32), C9(H9),
 C8(H8), C28(H28), C16(H16), C43(H43), C26(H26), C20(H20), C41(H41), C14(H14),
 C34(H34), C38(H38), C33(H33), C21(H21), C15(H15), C39(H39), C27(H27), C46(H46),
  C40(H40), C45(H45), C44(H44)
;
_shelx_res_checksum              26940
_olex2_submission_special_instructions 'No special instructions were received'