Structure and bonding in a cyclobutyl tris(pyrazolyl)boratoniobium complex and the variation in agostic behaviour with ring size in the series Tp(Me2)NbCl(c-C(n)H(2n-1))(MeC[triple bond]CMe), n = 3-6.
Besora, Maria; Maseras, Feliu; McGrady, John E.; Oulié, Pascal; Dinh, Duy Hai; Duhayon, Carine; Etienne, Michel; Dalton transactions (Cambridge, England : 2003)  (2006) 2362–2367; doi:10.1039/b516393e

data_7007015
_publ_section_title
;
 Structure and bonding in a cyclobutyl tris(pyrazolyl)boratoniobium
 complex and the variation in agostic behaviour with ring size in the
 series Tp(Me2)NbCl(c-C(n)H(2n-1))(MeC[triple bond]CMe), n = 3-6.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2362
_journal_page_last               2367
_journal_paper_doi               10.1039/b516393e
_journal_year                    2006
_chemical_formula_moiety         'C23 H35 B1 Cl1 N6 Nb1'
_chemical_formula_sum            'C23 H35 B Cl N6 Nb'
_chemical_formula_weight         534.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-01-19
_audit_creation_method           CRYSTALS_ver_12.24
_cell_angle_alpha                90
_cell_angle_beta                 96.613(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9098(8)
_cell_length_b                   15.8698(13)
_cell_length_c                   16.8149(13)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180
_cell_measurement_theta_max      24
_cell_measurement_theta_min      4
_cell_volume                     2626.8(4)
_computing_cell_refinement       'IPDS (Stoe & Cie, 1996)'
_computing_data_collection       'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_computing_molecular_graphics    'CAMERON (Watkin et al 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21329
_diffrn_reflns_theta_full        24.116
_diffrn_reflns_theta_max         24.116
_diffrn_reflns_theta_min         2.069
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.80
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1000
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         3239
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.007705
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.77 -0.101E-01 1.34
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0426
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0419
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                3239
_reflns_number_total             4144
_reflns_threshold_expression     I>2.50u(I)
_cod_data_source_file            b516393e.txt
_cod_data_source_block           CRYSTALS_cif
_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_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C23 H35 B1 Cl1 N6 Nb1'
_cod_database_code               7007015