Synthesis, Structures, and Dynamic Behavior of Intramolecularly Base-Stabilized Diphosphatetrylenes Containing a Five-Membered Chelate Ring
Izod, Keith; Stewart, John; Clegg, William; Harrington, Ross W.; Organometallics 29 (2010) 108–; doi:10.1021/om900854m

data_4067325
_publ_section_title
;
 Synthesis, Structures, and Dynamic Behavior of Intramolecularly
 Base-Stabilized Diphosphatetrylenes Containing a Five-Membered Chelate
 Ring
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              108
_journal_paper_doi               10.1021/om900854m
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C30 H58 Ge N2 P2 Si4'
_chemical_formula_sum            'C30 H58 Ge N2 P2 Si4'
_chemical_formula_weight         693.67
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.525(2)
_cell_angle_beta                 108.821(2)
_cell_angle_gamma                105.651(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0421(8)
_cell_length_b                   13.8295(11)
_cell_length_c                   15.5082(12)
_cell_measurement_reflns_used    13666
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.26
_cell_measurement_theta_min      2.30
_cell_volume                     1922.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11226
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.333
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         5014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.333
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0166P)^2^+3.7055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                4442
_reflns_number_total             5014
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om900854m_si_002.cif
_cod_data_source_block           5
_cod_database_code               4067325