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_7129786
_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         'C41 H31 P'
_chemical_formula_sum            'C41 H31 P'
_chemical_formula_weight         554.63
_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             2021-12-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-02-04 deposited with the CCDC.	2022-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                92.67(3)
_cell_angle_beta                 92.54(3)
_cell_angle_gamma                90.16(3)
_cell_formula_units_Z            2
_cell_length_a                   6.0760(12)
_cell_length_b                   12.198(2)
_cell_length_c                   19.747(4)
_cell_measurement_reflns_used    4789
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     1460.5(5)
_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)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1401
_diffrn_reflns_av_unetI/netI     0.1142
_diffrn_reflns_Laue_measured_fraction_full 0.931
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18649
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.671
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.064(8)
_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   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1032P)^2^+0.0906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1803
_refine_ls_wR_factor_ref         0.1903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3694
_reflns_number_total             4789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00698g2.cif
_cod_data_source_block           p-1
_cod_database_code               7129786
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.988
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.016) H7(0.027) H8(0.034) H9(0.031) H10(0.028) H11(0.023)
 H13(0.024) H14(0.033) H15(0.029) H16(0.025) H17(0.023) H19(0.033) H20(0.048)
 H21(0.049) H22(0.043) H23(0.03) H25(0.022) H26(0.025) H27(0.026) H28(0.023)
 H29(0.02) H31(0.023) H32(0.026) H33(0.026) H34(0.026) H35(0.021) H37(0.023)
 H38(0.028) H39(0.031) H40(0.026) H41(0.021)
 Fixed X: H1(0.845843) H7(0.275149) H8(0.299103) H9(0.613024) H10(0.905328)
 H11(0.880522) H13(0.484562) H14(0.686378) H15(1.033875) H16(1.176523)
 H17(0.972743) H19(0.214899) H20(0.186276) H21(0.488583) H22(0.818911)
 H23(0.853493) H25(0.524216) H26(0.290285) H27(-0.065412) H28(-0.182803)
 H29(0.048733) H31(0.813768) H32(0.761527) H33(0.423406) H34(0.129455)
 H35(0.178197) H37(0.598584) H38(0.813401) H39(1.157592) H40(1.282063)
 H41(1.069029)
 Fixed Y: H1(0.682763) H7(0.532046) H8(0.346759) H9(0.247133) H10(0.336015)
 H11(0.519413) H13(0.872863) H14(0.952199) H15(0.883489) H16(0.735301)
 H17(0.654813) H19(0.521874) H20(0.331104) H21(0.229588) H22(0.317287)
 H23(0.506725) H25(0.607754) H26(0.567575) H27(0.641023) H28(0.753)
 H29(0.79514) H31(0.952133) H32(1.110405) H33(1.198808) H34(1.125304)
 H35(0.966742) H37(1.04346) H38(1.179833) H39(1.137569) H40(0.957456)
 H41(0.819607)
 Fixed Z: H1(0.240338) H7(0.084058) H8(0.05171) H9(0.082598) H10(0.143515)
 H11(0.177309) H13(0.073413) H14(-0.008903) H15(-0.034655) H16(0.02344)
 H17(0.104114) H19(0.264545) H20(0.27048) H21(0.306393) H22(0.33906)
 H23(0.33112) H25(0.440039) H26(0.525597) H27(0.525659) H28(0.439595)
 H29(0.354029) H31(0.40258) H32(0.470344) H33(0.468296) H34(0.400237)
 H35(0.331732) H37(0.25155) H38(0.209807) H39(0.166217) H40(0.165607)
 H41(0.208419)
;
_shelx_res_checksum              85513
_olex2_submission_special_instructions 'No special instructions were received'