A New Nine-Membered Triphosphorus Macrocycle
Edwards, Peter G.; Whatton, Mark L.; Haigh, Robert; Organometallics 19 (2000) 2652–; doi:10.1021/om0002879

data_4077514
_publ_section_title
;
 A New Nine-Membered Triphosphorus Macrocycle
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              2652
_journal_paper_doi               10.1021/om0002879
_journal_volume                  19
_journal_year                    2000
_chemical_formula_moiety         '[C26 H42 Fe1 P3], PF6'
_chemical_formula_sum            'C26 H42 F6 Fe P4'
_chemical_formula_weight         648.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 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                 109.18(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.584(3)
_cell_length_b                   13.527(3)
_cell_length_c                   17.136(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      2.52
_cell_volume                     2974.0(12)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius,1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius,1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows(Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines(Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enraf Nonius FR590'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5590
_diffrn_reflns_theta_full        25.29
_diffrn_reflns_theta_max         25.29
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        6
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  0.8962
_exptl_absorpt_correction_T_min  0.5133
_exptl_absorpt_correction_type   DIFABS
_exptl_absorpt_process_details
;
Walker, N. & Stuart, D. 1983 Acta. Cryst. A39, 158-166 
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    'Calculated positions, riding model.'
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     757
_refine_ls_number_reflns         5590
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1032P)^2^+7.4288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1623
_refine_ls_wR_factor_ref         0.1737
_reflns_number_gt                5297
_reflns_number_total             5590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0002879.cif
_cod_data_source_block           s92
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2974.0(11)
_cod_original_sg_symbol_H-M      Pn
_cod_database_code               4077514