Carbonate formation within a nickel dimer: synthesis of a coordinatively unsaturated bis(mu-hydroxo) dinickel complex and its reactivity toward carbon dioxide.
Wikstrom, Jeffrey P.; Filatov, Alexander S.; Mikhalyova, Elena A.; Shatruk, Michael; Foxman, Bruce M.; Rybak-Akimova, Elena V; Dalton transactions (Cambridge, England : 2003) 39 (2010) 2504–2514; doi:10.1039/b916832j

data_7024423
_publ_section_title
;
 Carbonate formation within a nickel dimer: synthesis of a coordinatively
 unsaturated bis(mu-hydroxo) dinickel complex and its reactivity toward
 carbon dioxide.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2504
_journal_page_last               2514
_journal_paper_doi               10.1039/b916832j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C20 H29 Cl2 N5 Ni1 O9'
_chemical_formula_sum            'C20 H29 Cl2 N5 Ni O9'
_chemical_formula_weight         613.09
_chemical_name_systematic
;
bis(2-pyridylmethyl)tert-butylamine)
nickel perchlorate monohydrate diacetonotrile
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-05-20
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.686(2)
_cell_length_b                   14.934(3)
_cell_length_c                   32.606(7)
_cell_measurement_reflns_used    9335
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      5
_cell_volume                     5203.4(18)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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      120
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            37457
_diffrn_reflns_theta_full        30.020
_diffrn_reflns_theta_max         30.020
_diffrn_reflns_theta_min         5.053
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker AXS, 2006)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.08
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9735
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         7474
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.013964
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 5.65P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0845
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0845
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              45
_reflns_limit_l_min              0
_reflns_number_gt                6214
_reflns_number_total             7474
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.37
_oxford_diffrn_Wilson_scale      9.30
_oxford_refine_ls_r_factor_ref   0.0463
_oxford_refine_ls_scale          0.29857(19)
_oxford_reflns_number_all        7474
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'tufts in Pbca'
_cod_data_source_file            b916832j.txt
_cod_data_source_block           1*CH3CN*H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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 
;
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        'C20 H29 Cl2 N5 Ni1 O9'
_cod_database_code               7024423