Syntheses and crystal structures of lithium and niobium complexes containing a new type of monoanionic “scorpionate” ligand †
Otero, A.; Fernández-Baeza, J.; Tejeda, J.; Antiñolo, A.; Carrillo-Hermosilla, F.; Díez-Barra, E.; Lara-Sánchez, A.; Fernández-López, M.; Lanfranchi, M.; Pellinghelli, M. A.; Journal of the Chemical Society, Dalton Transactions  (1999) 3537–; doi:10.1039/a907505d

data_7027804
_publ_section_title
;
 Syntheses and crystal structures of lithium and niobium complexes
 containing a new type of monoanionic &#x201C;scorpionate&#x201D;
 ligand&#x200A;&#x2020;
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3537
_journal_paper_doi               10.1039/a907505d
_journal_year                    1999
_chemical_formula_moiety         'C21 H23 Cl2 N4 Nb O2, C H2 Cl2'
_chemical_formula_sum            'C22 H25 Cl4 N4 Nb O2'
_chemical_formula_weight         612.17
_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                 91.30(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.242(7)
_cell_length_b                   8.024(3)
_cell_length_c                   34.146(10)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      10
_cell_volume                     5271(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.468
_diffrn_measured_fraction_theta_max 0.468
_diffrn_measurement_device_type  'Philips PW 1100 diffractometer'
_diffrn_measurement_method       \q/2\q
_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  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0991
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7787
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.889
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.995
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         7677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.245
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1548
_reflns_number_gt                4042
_reflns_number_total             7677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            907505dsup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7027804