Selective carbon‒carbon bond cleavage of 2,2'-dibromotolane via photolysis of its appropriate (diphosphine)Pt0 complex in the solid state
Petzold, Holm; Weisheit, Thomas; Görls, Helmar; Breitzke, Hergen; Buntkowsky, Gerd; Escudero, Daniel; González, Leticia; Weigand, Wolfgang; Dalton Transactions  (2008) 1979–1981; doi:10.1039/B801230J

data_7003917
_publ_section_title
;
 Selective carbon--carbon bond cleavage of 2,2'-dibromotolane
 via photolysis of its appropriate (diphosphine)Pt0 complex in the
 solid state
;
_journal_issue                   15
_journal_name_full               'Dalton Transactions'
_journal_page_first              1979
_journal_page_last               1981
_journal_paper_doi               10.1039/B801230J
_journal_year                    2008
_chemical_formula_sum            'C44 H32 Br2 P2 Pt'
_chemical_formula_weight         977.55
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.710(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1456(4)
_cell_length_b                   22.1637(7)
_cell_length_c                   15.3986(4)
_cell_measurement_temperature    183(2)
_cell_volume                     3643.3(2)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23208
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    6.164
_exptl_absorpt_correction_T_max  0.6101
_exptl_absorpt_correction_T_min  0.2908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. R.H. Blessing, Acta Cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.193
_refine_diff_density_min         -2.345
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+15.3334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1463
_reflns_number_gt                6160
_reflns_number_total             8185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801230j.txt
_cod_data_source_block           FO2829?(Compound3)?
_cod_depositor_comments
;
Fixing incorrect symmetry operators. For the correct values, the
original paper at
http://pubs.rsc.org/en/Content/ArticleLanding/2008/DT/b801230j was
consulted.

Antanas Vaitkus
2013-03-06

Removing question marks from the following values:

 _audit_creation_method           SHELXL-97?
 _exptl_crystal_size_mid          0.04?
 _exptl_crystal_size_min          0.03?

 ...
 C29 0.091(8) 0.025(4) 0.051(5) 0.006(4) 0.021(5) -0.002(5)?
 C30 0.058(6) 0.047(6) 0.050(5) 0.019(4) 0.015(5) -0.006(5)?
 C31 0.057(6) 0.069(7) 0.035(5) 0.015(4) 0.028(4) 0.003(5)?

Removing extra question marks from disorder group values and from one
_geom_angle_publ_flag value.

Saulius Gra\<zulis
2014-05-06

;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7003917