Bis-BBN (9-borabicyclo[3.3.1]nonane) adduct of bis(diethylglyoximato)nickel(II)
Krivokapić, Alexander; Faiz, Jonathan A.; Anderson, Harry L.; Acta Crystallographica Section E 59 (2003) m748–m749; doi:10.1107/S1600536803017288

data_2202477
_publ_section_title
;
 Bis-BBN (9-borabicyclo[3.3.1]nonane) adduct of
 bis(diethylglyoximato)nickel(II)
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m748
_journal_page_last               m749
_journal_paper_doi               10.1107/S1600536803017288
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Ni (C28 H48 B2 N4 O4)]'
_chemical_formula_moiety         'C28 H48 B2 N4 Ni1 O4'
_chemical_formula_sum            'C28 H48 B2 N4 Ni O4'
_chemical_formula_weight         585.05
_chemical_melting_point          533.0(10)
_chemical_name_systematic
;
[2,9-bis(cyclooctane-1,5-diyl)-4,6,11,13-tetraethyl-1,3,8,10-tetraoxa-
4,7,11,14-tetraaza-2,9-diboracyclotetradecane-4,6,11,13-tetraene-
\k^4^N]nickel(II)
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 94.7398(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.40470(10)
_cell_length_b                   19.2467(2)
_cell_length_c                   10.5508(2)
_cell_measurement_reflns_used    3483
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1498.52(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001)'
_computing_data_reduction        DENZO/SCALEPACK
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Watkin et al., 2001)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Enraf--Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3497
_diffrn_reflns_theta_full        27.260
_diffrn_reflns_theta_max         27.397
_diffrn_reflns_theta_min         5.336
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             628.000
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.28
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0376
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2934
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          <0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994)
W = [weight][1-(\dF/6\sF)^2^]^2^, with 2.03, 0.469E-1 and 1.40
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0349
_refine_ls_wR_factor_gt          0.0314
_refine_ls_wR_factor_ref         0.0314
_reflns_number_gt                2934
_reflns_number_total             3386
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            ci6244.cif
_cod_data_source_block           I
_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 

The following automatic conversions were performed:

'_chemical_melting_point' value '532-534 K' was changed to
'533.0(10)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '532-534 K' was changed to
'533.0(10)' - the average value was taken and precision was
estimated.

'_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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C28 H48 B2 N4 Ni1 O4'
_cod_database_code               2202477
_cod_database_fobs_code          2202477