Reactions of alkynes with phosphido niobocenes: a combined experimental and theoretical study.
Antiñolo, Antonio; García-Yuste, Santiago; Solera, Isabel Lopez; Otero, Antonio; Pérez-Flores, Juan Carlos; Reguillo-Carmona, Rebeca; Villaseñor, Elena; Santos, Eva; Zuidema, Erik; Bo, Carles; Dalton transactions (Cambridge, England : 2003) 39 (2010) 1962–1971; doi:10.1039/b918298e

data_7024548
_publ_section_title
;
 Reactions of alkynes with phosphido niobocenes: a combined experimental
 and theoretical study.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1962
_journal_page_last               1971
_journal_paper_doi               10.1039/b918298e
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C51.5 H59.5 N Nb O2 P Si2'
_chemical_formula_weight         904.56
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.144(3)
_cell_angle_beta                 102.049(3)
_cell_angle_gamma                108.324(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7939(5)
_cell_length_b                   12.2093(6)
_cell_length_c                   19.3334(9)
_cell_measurement_temperature    100(2)
_cell_volume                     2345.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SHELXTL'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0637
_diffrn_reflns_av_sigmaI/netI    0.0834
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25036
_diffrn_reflns_theta_full        25.90
_diffrn_reflns_theta_max         25.90
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.72325
_exptl_absorpt_correction_type   Semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Prismatic
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Orange
_exptl_crystal_F_000             951
_exptl_crystal_size_max          0.352
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.653
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         9067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.653
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1732P)^2^+11.2598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1792
_reflns_number_gt                6608
_reflns_number_total             9067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b918298e.txt
_cod_data_source_block           compound_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2345.39(19)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C51.50 H59.50 N Nb O2 P Si2'
_cod_database_code               7024548