Calcium fluoride incorporated in soluble organometallics: adduct formation and solution dynamics
Demsar, Alojz; Pevec, Andrej; Petriček, Saša; Golič, Ljubo; Petrič, Andrej; Björgvinsson, Már; Roesky, Herbert W.; Journal of the Chemical Society, Dalton Transactions  (1998) 4043–; doi:10.1039/a806209i

data_7027048
_publ_contact_author
;
    Dr.Alojz Demsar
     University of Ljubljana
     Faculty of Chemistry and Chemical Technology
     Askerceva 5
     1000 Ljubljana
     Slovenia
 
;
_publ_section_title
;
 Calcium fluoride incorporated in soluble organometallics: adduct
 formation and solution dynamics
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4043
_journal_paper_doi               10.1039/a806209i
_journal_year                    1998
_chemical_formula_moiety         \(C5Me4Et)2Ti2F7\2Ca(OP(NMe2)3)
_chemical_formula_structural     \(C5Me4Et)2Ti2F7\4Ca2(OP(NMe2)3)2
_chemical_formula_sum            'C50 H86 Ca F14 N3 O P Ti4'
_chemical_formula_weight         1273.4
_chemical_name_systematic
;bis\bis(1-ethyl-2,3,4,5-tetramethyl-
2,4-cyclopentadien-1-il)tri-m-fluorotetrafluorodititanato(IV)-F,F',F'',
F'''\hexamethylphosphoramidecalcium 
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   fourr
_audit_creation_date             98-06-29
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                90.00000
_cell_angle_beta                 113.000(7)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   27.768(2)
_cell_length_b                   21.176(2)
_cell_length_c                   22.747(2)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    293
_cell_measurement_theta_max      14.95
_cell_measurement_theta_min      9.98
_cell_volume                     12312.3(19)
_computing_data_reduction        xtal_DIFDAT_SORTRF_ADDREF
_computing_molecular_graphics    xtal
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    sir92
_diffrn_ambient_temperature      293
_diffrn_measurement_device       CAD4
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         xray_tube
_diffrn_radiation_type           'Mo K \a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  .016
_diffrn_reflns_av_sigmaI/netI    .042
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            .311990+05
_diffrn_reflns_reduction_process perpendicular_monochr_Lp
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        -59.4
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.678
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_F_000             5312
_exptl_crystal_size_max          1.05
_exptl_crystal_size_mid          0.84
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.5
_refine_diff_density_min         -2.2
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       13(1712)
_refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   4.817
_refine_ls_goodness_of_fit_obs   .999
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1334
_refine_ls_number_reflns         .106240+05
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .198
_refine_ls_R_factor_obs          .056
_refine_ls_shift/esd_max         .001
_refine_ls_shift/esd_mean        .0001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .105
_refine_ls_wR_factor_obs         .056
_reflns_d_resolution_high        .757
_reflns_d_resolution_low         16.307
_reflns_limit_h_max              36
_reflns_limit_h_min              0
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              -30
_reflns_number_observed          .106350+05
_reflns_number_total             .295850+05
_reflns_observed_criterion       refl_observed_if_F____>_2.5__sigma(F___)
_cod_data_source_file            806209Isup1.cif
_cod_data_source_block           ap
_cod_original_cell_volume        12312(2)
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_original_sg_symbol_H-M      p_1_21/c_1
_cod_original_formula_sum        C50H86CaF14N3OPTi4
_cod_database_code               7027048