Antimony(i) →Pd(ii) complexes with the (μ-Sb)Pd<sub>2</sub> coordination framework.
Kořenková, Monika; Hejda, Martin; Jirásko, Robert; Block, Theresa; Uhlík, Filip; Jambor, Roman; RůŽička, Aleš; Pöttgen, Rainer; Dostál, Libor; Dalton transactions (Cambridge, England : 2003) 48 (2019) 11912–11920; doi:10.1039/c9dt02340b

data_7700416
_publ_section_title
;
 Antimony(i) \\rightarrow Pd(ii) complexes with the (\m-Sb)Pd<sub>2</sub>
 coordination framework.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11912
_journal_page_last               11920
_journal_paper_doi               10.1039/c9dt02340b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C26 H33 F6 N2 O4 Pd2 Sb, C6 H6'
_chemical_formula_sum            'C32 H39 F6 N2 O4 Pd2 Sb'
_chemical_formula_weight         964.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'APEX3 v2016.5-0'
_audit_update_record
;
2019-04-05 deposited with the CCDC.    2019-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3001(13)
_cell_length_b                   10.5868(6)
_cell_length_c                   18.5561(14)
_cell_measurement_reflns_used    31675
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1
_cell_volume                     3595.0(4)
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1584
_diffrn_reflns_av_unetI/netI     0.1340
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30074
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.901
_diffrn_reflns_theta_min         2.479
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.804
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details
;
 Flack x determined using 1991 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         8073
_refine_ls_number_restraints     551
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0227P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.913
_reflns_number_gt                5563
_reflns_number_total             8073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02340b2.cif
_cod_data_source_block           ld181210Sb2
_cod_depositor_comments
'Adding full bibliography for 7700416--7700419.cif.'
_cod_database_code               7700416
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.625
;
_shelxl_version_number           2013-4
_shelx_res_checksum              58950