Thermal and Photochemical Ring-Bromination in Naphthyl-, Naphthdiyl-, and Dicarboximideperyl-Platinum Complexes
Raphael Karikachery, Alice; Masjedi, Mehdi; Sharp, Paul R.; Organometallics 34 (2015) 1635–; doi:10.1021/om501322f

data_4085702
_publ_section_title
;
 Thermal and Photochemical Ring-Bromination in Naphthyl-, Naphthdiyl-, and
 Dicarboximideperyl-Platinum Complexes
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1635
_journal_paper_doi               10.1021/om501322f
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C34 H64 Br4 P4 Pt2'
_chemical_formula_sum            'C34 H64 Br4 P4 Pt2'
_chemical_formula_weight         1306.55
_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'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1377(10)
_cell_length_b                   16.7133(13)
_cell_length_c                   19.9374(16)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.1
_cell_measurement_theta_min      2.2
_cell_volume                     4377.7(6)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51041
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_min         1.590
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    10.204
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 G\"ottingen, Germany).
;
_exptl_crystal_colour            Pale_Yellow
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.962
_refine_diff_density_min         -2.102
_refine_diff_density_rms         0.196
_refine_ls_abs_structure_details
;
 Flack x determined using 3340 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         10016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0421P)^2^+14.2377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.807
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.991
_reflns_number_gt                8456
_reflns_number_total             10016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501322f_si_002.cif
_cod_data_source_block
'[trans-Pt(PEt3)2(Br)]2(6,7-Br2-1,4-naphthdiyl)_13'
_cod_depositor_comments
'Adding full bibliography for 4085699--4085702.cif.'
_cod_database_code               4085702
_shelx_estimated_absorpt_t_min   0.071
_shelx_estimated_absorpt_t_max   0.686
_shelxl_version_number           2014-3
_shelx_res_checksum              2687
_shelx_hkl_checksum              89120