Photoreductive Elimination of Chlorine from Antimony in an [SbPd]<sup>VII</sup> Complex.
Sahu, Sumit; Gabbaï, François P; Journal of the American Chemical Society 139 (2017) 5035–5038; doi:10.1021/jacs.7b01977

data_4131253
_publ_section_title
;
 Photoreductive Elimination of Chlorine from Antimony in an
 [SbPd]<sup>VII</sup> Complex.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5035
_journal_page_last               5038
_journal_paper_doi               10.1021/jacs.7b01977
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C36 H28 Cl5 P2 Pd Sb'
_chemical_formula_sum            'C36 H28 Cl5 P2 Pd Sb'
_chemical_formula_weight         927.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1833(5)
_cell_length_b                   14.0387(5)
_cell_length_c                   18.8114(7)
_cell_measurement_reflns_used    9590
_cell_measurement_temperature    110
_cell_measurement_theta_max      28.95
_cell_measurement_theta_min      2.38
_cell_volume                     3481.5(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11078
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.636
_diffrn_reflns_theta_min         1.810
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.795
_exptl_absorpt_correction_T_max  0.4935
_exptl_absorpt_correction_T_min  0.4058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0994 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.8223.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_description       plate
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.261
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         10705
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0308P)^2^+4.5133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                9478
_reflns_number_total             10705
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b01977_si_003.cif
_cod_data_source_block           2
_cod_database_code               4131253
_shelx_estimated_absorpt_t_max   0.715
_shelx_estimated_absorpt_t_min   0.715
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55(2) 0.45(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C17(H17), C16(H16), C15(H15), C14(H14), C12(H12), C11(H11),
 C10(H10), C9(H9), C8(H8), C5(H5), C4(H4), C3(H3), C2(H2), C29(H29), C28(H28),
 C27(H27), C26(H26), C23(H23), C22(H22), C21(H21), C20(H20), C36(H36), C35(H35),
  C34(H34), C33(H33), C32(H32), C30(H30)
;
_shelx_res_checksum              76290
_shelx_hkl_checksum              81326
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'