Stereoelectronic effects in a homologous series of bidentate cyclic phosphines. A clear correlation of hydroformylation catalyst activity with ring size
Haddow, Mairi F.; Middleton, Ann J.; Orpen, A. Guy; Pringle, Paul G.; Papp, Rainer; Dalton Transactions  (2009) 202–209; doi:10.1039/B815056G

data_7000169
_publ_section_title
;
 Stereoelectronic effects in a homologous series of bidentate cyclic
 phosphines. A clear correlation of hydroformylation catalyst activity
 with ring size
;
_journal_issue                   1
_journal_name_full               'Dalton Transactions'
_journal_page_first              202
_journal_page_last               209
_journal_paper_doi               10.1039/B815056G
_journal_year                    2009
_chemical_formula_moiety         'C15 H30 Cl2 P2 Pt'
_chemical_formula_sum            'C15 H30 Cl2 P2 Pt'
_chemical_formula_weight         538.32
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 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                 92.05(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   34.324(7)
_cell_length_b                   6.3850(13)
_cell_length_c                   12.625(3)
_cell_measurement_reflns_used    5098
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.498
_cell_measurement_theta_min      2.376
_cell_volume                     2765.1(10)
_computing_cell_refinement       'Bruker SMART V5.054 (Bruker, 1998)'
_computing_data_collection       'Bruker SMART V5.054 (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT V6.02 (Bruker, 1999)'
_computing_molecular_graphics    'Bruker SHELXTL V6.14 (Bruker AXS, 2003)'
_computing_publication_material  'Bruker SHELXTL V6.14 (Bruker AXS, 2003)'
_computing_structure_refinement  'SHELXL V6.12 (Bruker 2001)'
_computing_structure_solution    'SHELXS V6.12 (Bruker 2001)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28297
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.19
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.065
_exptl_absorpt_correction_T_max  0.620000
_exptl_absorpt_correction_T_min  0.335706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick,2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.763
_refine_diff_density_min         -1.574
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         12421
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+4.4274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0693
_reflns_number_gt                11954
_reflns_number_total             12421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815056g.txt
_cod_data_source_block           4c_ajm193sad
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               7000169