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_4131252
_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 Cl3 P2 Pd Sb'
_chemical_formula_sum            'C36 H28 Cl3 P2 Pd Sb'
_chemical_formula_weight         857.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 94.2177(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6603(4)
_cell_length_b                   12.7003(3)
_cell_length_c                   17.8348(4)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    110
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.36
_cell_volume                     3311.67(14)
_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 0.997
_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  0.0575
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            70051
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.585
_diffrn_reflns_theta_min         1.737
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.723
_exptl_absorpt_correction_T_max  0.4935
_exptl_absorpt_correction_T_min  0.4266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0851 before and 0.0593 after correction.
The Ratio of minimum to maximum transmission is 0.8644.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0206P)^2^+4.0224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6367
_reflns_number_total             7657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b01977_si_002.cif
_cod_data_source_block           1
_cod_database_code               4131252
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.029) H4(0.032) H5(0.032) H6(0.029) H8(0.028) H9(0.033)
 H10(0.031) H11(0.032) H12(0.028) H14(0.034) H15(0.042) H16(0.043) H17(0.043)
 H18(0.032) H21(0.027) H22(0.03) H23(0.033) H24(0.029) H26(0.027) H27(0.032)
 H28(0.032) H29(0.033) H30(0.03) H32(0.027) H33(0.033) H34(0.036) H35(0.039)
 H36(0.031)
 Fixed X: H3(0.3302) H4(0.3703) H5(0.2677) H6(0.1216) H8(0.239) H9(0.2067)
 H10(0.0904) H11(0.0034) H12(0.0343) H14(0.2771) H15(0.4161) H16(0.4923)
 H17(0.4339) H18(0.2962) H21(-0.2649) H22(-0.3366) H23(-0.271) H24(-0.1314)
 H26(-0.1314) H27(-0.2386) H28(-0.3483) H29(-0.3559) H30(-0.2503) H32(-0.0878)
 H33(-0.0611) H34(-0.0427) H35(-0.0513) H36(-0.0761)
 Fixed Y: H3(0.0121) H4(-0.0326) H5(-0.0133) H6(0.0521) H8(-0.1203) H9(-
 0.2717) H10(-0.273) H11(-0.1232) H12(0.0286) H14(0.2731) H15(0.3317)
 H16(0.2354) H17(0.0773) H18(0.0158) H21(0.3584) H22(0.3263) H23(0.2172)
 H24(0.1373) H26(0.0943) H27(0.0254) H28(0.1332) H29(0.3082) H30(0.3781)
 H32(0.4371) H33(0.6163) H34(0.7177) H35(0.6413) H36(0.4626)
 Fixed Z: H3(0.2478) H4(0.1292) H5(0.0264) H6(0.0412) H8(0.3146) H9(0.3785)
 H10(0.459) H11(0.473) H12(0.4079) H14(0.3008) H15(0.3547) H16(0.4488)
 H17(0.4867) H18(0.4311) H21(0.2056) H22(0.0886) H23(0.0045) H24(0.0374)
 H26(0.3514) H27(0.4261) H28(0.4716) H29(0.4368) H30(0.3609) H32(0.4093)
 H33(0.4211) H34(0.3161) H35(0.199) H36(0.1855)
;
_shelx_res_checksum              62307
_shelx_hkl_checksum              44448
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'