Mono-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) m745–m747; doi:10.1107/S160053680301729X

data_2202476
_publ_section_title
;
 Mono-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              m745
_journal_page_last               m747
_journal_paper_doi               10.1107/S160053680301729X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Ni (C20 H35 B N4 O4)]'
_chemical_formula_moiety         'C20 H35 B N4 Ni O4'
_chemical_formula_sum            'C20 H35 B N4 Ni O4'
_chemical_formula_weight         465.04
_chemical_melting_point          465.0(10)
_chemical_name_systematic
;
[7-(cyclooctane-1,5-diyl)-2,3,11,12-tetraethyl-6,8-dioxa-5,9-diaza-7-
boratridecane-1,13-dicarbaldehyde dioximato-\k^4^N]nickel(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                79.4462(6)
_cell_angle_beta                 70.0605(7)
_cell_angle_gamma                69.4812(11)
_cell_formula_units_Z            4
_cell_length_a                   11.5210(2)
_cell_length_b                   14.8794(2)
_cell_length_c                   14.9455(3)
_cell_measurement_reflns_used    8108
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      4
_cell_volume                     2249.76(7)
_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 0.969
_diffrn_measured_fraction_theta_max 0.953
_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  0.01
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16886
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.425
_diffrn_reflns_theta_min         4.099
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             992.000
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0385
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         7437
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0298
_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 0.901, 0.532 and 0.614
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0455
_refine_ls_wR_factor_gt          0.0375
_refine_ls_wR_factor_ref         0.0375
_reflns_number_gt                7437
_reflns_number_total             9767
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            ci6243.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 '464-466 K' was changed to
'465.0(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 '464-466 K' was changed to
'465.0(10)' - the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Triclinic' changed to
'triclinic' 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_database_code               2202476
_cod_database_fobs_code          2202476