Synthesis and Reactions of Ethynylferrocene-Derived Fluoro- and Chlorocyclotriphosphazenes
Karunesh Keshav; Nem Singh; Anil J. Elias; Inorganic Chemistry 49 (2010) 5753–5765; doi:10.1021/ic100703h

data_4315843
_publ_contact_author_address
;DEPARTMENT OF CHEMISTRY
INDIAN INSTITUTE OF TECHNOLOGY DELHI
HAUZ KHAS, NEW DELHI 110016
INDIA
;
_publ_contact_author_email       elias@chemistry.iitd.ac.in
_publ_contact_author_fax         +91-11-2658????
_publ_contact_author_name        'Dr.Anil J. Elias'
_publ_contact_author_phone       +91-11-2659????
_publ_section_title
;
 Synthesis and Reactions of Ethynylferrocene-Derived Fluoro- and
 Chlorocyclotriphosphazenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5753
_journal_page_last               5765
_journal_paper_doi               10.1021/ic100703h
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C24 H18 F4 Fe2 N3 P3'
_chemical_formula_sum            'C24 H18 F4 Fe2 N3 P3'
_chemical_formula_weight         629.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 130.422(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.469(4)
_cell_length_b                   19.649(4)
_cell_length_c                   10.899(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.50
_cell_measurement_theta_min      2.02
_cell_volume                     2522.0(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10252
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264.0
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+10.4544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                1800
_reflns_number_total             1851
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100703h_si_002_03.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2522.0(10)
_cod_original_sg_symbol_Hall     -C2yc
_cod_database_code               4315843