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_4334403
_publ_contact_author
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        Martin Nieger
        Laboratory of Inorganic Chemistry
        Department of Chemistry
        Universitity of Helsinki
        P.O. Box 55
        FIN-00014 University of Helsinki
        Finland
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_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
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 Conformationally Constrained N-Heterocyclic Phosphine-Diimine with Dual
 Functionality
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_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         'C15 H18 N5 O5 P W'
_chemical_formula_sum            'C15 H18 N5 O5 P W'
_chemical_formula_weight         563.16
_chemical_name_systematic
; 
 9-Dimethylamino-4,4',8a,8a'-tetraaza-9-phospha-2,3,6,7,8,8a,9,9a-
 octahydro-1H-fluorene-tungstenpentacarbonyl 
;
_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                 91.04(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.670(1)
_cell_length_b                   12.722(1)
_cell_length_c                   31.666(3)
_cell_measurement_reflns_used    74
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     3895.0(6)
_computing_cell_refinement       EVALCCD
_computing_data_collection       Collect
_computing_data_reduction        EVALCCD
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 1 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            6671
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    6.050
_exptl_absorpt_correction_T_max  0.5818
_exptl_absorpt_correction_T_min  0.3622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'pale rosa'
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plates
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.878
_refine_diff_density_min         -2.869
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         6671
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0300P)^2^+300.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1830
_refine_ls_wR_factor_ref         0.1852
_reflns_number_gt                6223
_reflns_number_total             6671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400261w_si_002.cif
_cod_data_source_block           dg112_tw_compound_7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4334403