Synthesis and Structural Properties of Aza[n]helicene Platinum Complexes: Control of Cis and Trans Stereochemistry.
Mendola, Daniele; Saleh, Nidal; Hellou, Nora; Vanthuyne, Nicolas; Roussel, Christian; Toupet, Loïc; Castiglione, Franca; Melone, Federica; Caronna, Tullio; Fontana, Francesca; Martí-Rujas, Javier; Parisini, Emilio; Malpezzi, Luciana; Mele, Andrea; Crassous, Jeanne; Inorganic chemistry 55 (2016) 2009–2017; doi:10.1021/acs.inorgchem.5b02276

data_4346876
_publ_section_title
;
 Synthesis and Structural Properties of Aza[n]helicene Platinum Complexes:
 Control of Cis and Trans Stereochemistry.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2009
_journal_page_last               2017
_journal_paper_doi               10.1021/acs.inorgchem.5b02276
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C44 H32 Cl4 N P Pt'
_chemical_formula_weight         942.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                61.388(6)
_cell_angle_beta                 69.548(5)
_cell_angle_gamma                79.328(5)
_cell_formula_units_Z            2
_cell_length_a                   10.6352(5)
_cell_length_b                   14.6650(9)
_cell_length_c                   14.7018(8)
_cell_measurement_reflns_used    11915
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.61
_cell_volume                     1885.6(2)
_computing_cell_refinement
'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.37.35'
_computing_data_collection
'CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.37.35'
_computing_data_reduction
'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.37.35'
_computing_molecular_graphics    'MERCURY 3.3(CCDC, 2014)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-97_(Altomare & al., 1999)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 16.1852
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'CCD Saphire 3 Xcalibur'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0892
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12736
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.612
_exptl_absorpt_coefficient_mu    4.080
_exptl_absorpt_correction_T_max  0.83853
_exptl_absorpt_correction_T_min  0.59876
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'Alcock(1970) crystallographic computing,p271'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       prism
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.059
_refine_diff_density_max         6.261
_refine_diff_density_min         -2.917
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0617
_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^)+(0.1023P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5918
_reflns_number_total             7586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02276_si_004.cif
_cod_data_source_block           shelx
_cod_database_code               4346876
_shelxl_version_number           2014/6
_shelx_res_checksum              59923
_shelx_hkl_checksum              30204