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_7129787
_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         'C70 H50 Sm, 2(C7 H8)'
_chemical_formula_sum            'C84 H66 Sm'
_chemical_formula_weight         1225.71
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-20
_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                90
_cell_angle_beta                 95.03(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.481(2)
_cell_length_b                   17.845(4)
_cell_length_c                   16.322(3)
_cell_measurement_reflns_used    5119
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     3041.0(11)
_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 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'ADSC Quantum 315r'
_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  0.2739
_diffrn_reflns_av_unetI/netI     0.1712
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31042
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.035
_diffrn_reflns_theta_max         25.035
_diffrn_reflns_theta_min         1.694
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.248
_refine_diff_density_min         -2.921
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5119
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1563
_refine_ls_R_factor_gt           0.1207
_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^)+(0.1760P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2836
_refine_ls_wR_factor_ref         0.3250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2555
_reflns_number_total             5119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00698g2.cif
_cod_data_source_block           3
_cod_database_code               7129787
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.905
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C23(H23), C25(H25), C11(H11), C13(H13), C17(H17), C22(H22),
 C31(H31), C19(H19), C28(H28), C27(H27), C32(H32), C26(H26), C35(H35), C10(H10),
  C16(H16), C14(H14), C21(H21), C34(H34), C7(H7), C33(H33), C20(H20), C15(H15),
 C9(H9), C8(H8)
;
_shelx_res_checksum              72690
_olex2_submission_special_instructions 'No special instructions were received'