Conformationally Constrained N-Heterocyclic Phosphine-Diimine with Dual Functionality
Georgios Mourgas; Martin Nieger; Daniela Förster; Dietrich Gudat; Inorganic Chemistry 52 (2013) 4104–4112; doi:10.1021/ic400261w

data_4334405
_publ_contact_author
;
        Martin Nieger
        Laboratory of Inorganic Chemistry
        Department of Chemistry
        Universitity of Helsinki
        P.O. Box 55
        FIN-00014 University of Helsinki
        Finland
;
_publ_contact_author_email       martin.nieger@helsinki.fi
_publ_contact_author_fax         ++358-9-19150198
_publ_contact_author_phone       ++358-9-19150192
_publ_section_title
;
 Conformationally Constrained N-Heterocyclic Phosphine-Diimine with Dual
 Functionality
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4104
_journal_page_last               4112
_journal_paper_doi               10.1021/ic400261w
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C10 H18 As Cl N5 P, As Cl3,C H2 Cl2, 2(Cl)'
_chemical_formula_sum            'C22 H40 As4 Cl16 N10 P2'
_chemical_formula_weight         1373.46
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 93.339(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9973(2)
_cell_length_b                   19.5332(5)
_cell_length_c                   12.3096(3)
_cell_measurement_reflns_used    5845
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      0.4
_cell_volume                     2399.73(10)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'SHELXL 97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-NONIUS APEXII'
_diffrn_measurement_method       'rotation in phi and omega, 0.9 deg.'
_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  0.1372
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            47436
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         4.14
_exptl_absorpt_coefficient_mu    3.752
_exptl_absorpt_correction_T_max  0.7736
_exptl_absorpt_correction_T_min  0.5058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'mulabs (Platon, c.f. Blessing, 1995)'
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         5692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+16.7040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                4099
_reflns_number_total             5692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400261w_si_004.cif
_cod_data_source_block           gm03_m
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4334405