Monocyclopentadienyl complexes of niobium, tantalum and tungsten containing heterodifunctional P,O ligands
Morise, Xavier; Green, Malcolm L. H.; Braunstein, Pierre; Rees, Leigh H.; Vei, Ino C.; New Journal of Chemistry 27 (2003) 32–38; doi:10.1039/b202983a

data_7050396
_publ_section_title
;
 Monocyclopentadienyl complexes of niobium, tantalum and tungsten
 containing heterodifunctional P,O ligands
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              32
_journal_page_last               38
_journal_paper_doi               10.1039/b202983a
_journal_volume                  27
_journal_year                    2003
_chemical_formula_moiety         ' C30 H31 Cl3 O1 P1 Ta1 '
_chemical_formula_sum            'C30 H31 Cl3 O P Ta'
_chemical_formula_weight         725.86
_chemical_melting_point          ?
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   42.5519(5)
_cell_length_b                   42.5519(5)
_cell_length_c                   8.7407(5)
_cell_measurement_reflns_used    6889
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     13706.1(8)
_computing_cell_refinement
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics    'CAMERON (Watkin et al 1996)'
_computing_publication_material  'CRYSTALS (Watkin et al 2001)'
_computing_structure_refinement  'CRYSTALS (Watkin et al 2001)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Enraf Nonius Kappa CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6943
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         5.16
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.945
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             6431.330
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.34
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0695
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5794
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.007337
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 
1.81    -.961     1.15    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0298
_reflns_limit_h_max              26
_reflns_limit_h_min              -55
_reflns_limit_k_max              55
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                5794
_reflns_number_total             6943
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            b202983a.txt
_cod_data_source_block           CRYSTALS_cif_1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal ' changed to 'trigonal' according
to '/home/adriana/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        13706.1
_cod_original_sg_symbol_H-M      'R -3 '
_cod_original_formula_sum        ' C30 H31 Cl3 O1 P1 Ta1 '
_cod_database_code               7050396