C‒H and C‒C agostic interactions in cycloalkyl tris(pyrazolyl)boratoniobium complexes
Joëlle Jaffart; Marcus L. Cole; Michel Etienne; Meike Reinhold; John E. McGrady; Feliu Maseras; Dalton Trans.  (2003) 4057–4064; doi:10.1039/b305296f

data_7013175
_publ_section_title
;
 C--H and C--C agostic interactions in cycloalkyl
 tris(pyrazolyl)boratoniobium complexes
;
_journal_issue                   21
_journal_name_full               'Dalton Trans.'
_journal_page_first              4057
_journal_page_last               4064
_journal_paper_doi               10.1039/b305296f
_journal_year                    2003
_chemical_compound_source
;
?
;
_chemical_formula_moiety         'C24 H37 Nb1 Cl1 N6 B1, 0.5 C7 H8'
_chemical_formula_sum            'C27.5 H41 B Cl N6 Nb'
_chemical_formula_weight         594.84
_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   'Geometric or located (Fourier difference)'
_atom_sites_solution_primary     'Direct_Methods SIR92'
_cell_angle_alpha                90
_cell_angle_beta                 96.52(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   39.571(5)
_cell_length_b                   13.711(1)
_cell_length_c                   10.669(1)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    160
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      1.6
_cell_volume                     5751.1(10)
_computing_cell_refinement       ' STOE IPDS '
_computing_data_collection       ' STOE IPDS '
_computing_data_reduction
;
STOE XRED
;
_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      160
_diffrn_measurement_device       ' STOE IPDS '
_diffrn_measurement_method       '\f rotation'
_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       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3734
_diffrn_reflns_theta_max         27.6
_diffrn_reflns_theta_min         1.6
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.54
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' orange '
_exptl_crystal_density_diffrn    1.37
_exptl_crystal_description       ' box '
_exptl_crystal_F_000             2354
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_obs   1.1384
_refine_ls_hydrogen_treatment
;
H atoms placed geometrically after each cycle, except H1 and H11
located and refined isotropically
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         2705
_refine_ls_R_factor_obs          0.0340
_refine_ls_shift/esd_max         0.001378
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
w = w'[1-(?F/6?(F))2]2. w' = 1/?(r=1,3)ArTr(x) where Ar are the
coefficients for the Chebyshev polynomial Tr(x) with x = Fc/Fc(max)
(Carruthers & Watkin, 1979)
coef 1.76, -2.34, 1.57, -0.939, 0.220
;
_refine_ls_wR_factor_obs         0.0349
_reflns_limit_h_max              41
_reflns_limit_h_min              -42
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_observed          2705
_reflns_number_total             16617
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            b305296f.txt
_cod_data_source_block           compound1
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5751(1)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               7013175