Niobium‒η-cyclopentadienyl compounds with imido and amido ligands derived from 2,6-dimethylaniline
Humphries, Martin J.; Green, Malcolm L. H.; Douthwaite, Richard E.; Rees, Leigh H.; Journal of the Chemical Society, Dalton Transactions  (2000) 4555–; doi:10.1039/b007178l

data_7010226
_publ_section_title
;
 Niobium--\h-cyclopentadienyl compounds with imido and amido ligands
 derived from 2,6-dimethylaniline
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4555
_journal_paper_doi               10.1039/b007178l
_journal_year                    2000
_chemical_formula_moiety         ' C13 H14 Cl2 N1 Nb1 '
_chemical_formula_sum            'C13 H14 Cl2 N Nb'
_chemical_formula_weight         348.07
_chemical_melting_point          ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             99-05-31
_audit_creation_method           CRYSTALS_ver_07-07-97
_cell_angle_alpha                90.
_cell_angle_beta                 103.61(2)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   8.775(2)
_cell_length_b                   12.804(2)
_cell_length_c                   12.648(2)
_cell_measurement_reflns_used    7157
_cell_measurement_temperature    180
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      0
_cell_volume                     1381.2(5)
_computing_cell_refinement
;
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
DIP2000 software 'Xpress' (MAC Science, 1989)
;
_computing_data_reduction
; 
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce, 1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      180
_diffrn_measurement_device_type
;
Enraf-nonius DIP2000
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7157
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.20
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.67
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' box '
_exptl_crystal_F_000             688.18
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.96
_refine_diff_density_min         -0.85
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_obs   1.0881
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2682
_refine_ls_R_factor_obs          0.0508
_refine_ls_shift/su_max          0.000117
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
3.05 1.64 2.34
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0533
_reflns_number_observed          2682
_reflns_number_total             2879
_reflns_observed_criterion       3.00\s(I)
_cod_data_source_file            b007178l.txt
_cod_data_source_block           structure1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
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        1381.1
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C13 H14 Cl2 N1 Nb1 '
_cod_database_code               7010226