Dynamic behaviour attributed to chiral carbohydrate substituents of N-heterocyclic carbene ligands in square planar nickel complexes.
Shibata, Teppei; Ito, Satoru; Doe, Matsumi; Tanaka, Rika; Hashimoto, Hideki; Kinoshita, Isamu; Yano, Shigenobu; Nishioka, Takanori; Dalton transactions (Cambridge, England : 2003) 40 (2011) 6778–6784; doi:10.1039/c0dt01833c

data_7016025
_publ_section_title
;
 Dynamic behaviour attributed to chiral carbohydrate substituents of
 N-heterocyclic carbene ligands in square planar nickel complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6778
_journal_page_last               6784
_journal_paper_doi               10.1039/c0dt01833c
_journal_volume                  40
_journal_year                    2011
_chemical_absolute_configuration rmad
_chemical_formula_moiety         '(C48 H56 Br2 N4 Ni O18), 0.5(C7 H8)'
_chemical_formula_sum            'C51.5 H60 Br2 N4 Ni O18'
_chemical_formula_weight         1241.56
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.9010(6)
_cell_length_b                   23.3218(8)
_cell_length_c                   23.7857(7)
_cell_measurement_reflns_used    7031
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.0112
_cell_volume                     11594.3(6)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2001)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
scan:
Number of images: 900
Slice: -80.0000 - 100.0000
Image width: 0.2000
Exp time: 5.0000
Rotation axis: Phi
Omega: 0.0000
Chi: 0.0000
Phi: 0.0000
XTD: 55.2092
2theta: 24.8033
scan:
Number of images: 300
Slice: -15.0000 - 45.0000
Image width: 0.2000
Exp time: 5.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 0.0000
XTD: 55.2092
2theta: 24.8033
scan:
Number of images: 300
Slice: -15.0000 - 45.0000
Image width: 0.2000
Exp time: 5.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 90.0000
XTD: 55.2092
2theta: 24.8033
scan:
Number of images: 300
Slice: -15.0000 - 45.0000
Image width: 0.2000
Exp time: 5.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 180.0000
XTD: 55.2092
2theta: 24.8033
scan:
Number of images: 300
Slice: -15.0000 - 45.0000
Image width: 0.2000
Exp time: 5.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 270.0000
XTD: 55.2092
2theta: 24.8033

;
_diffrn_measurement_device       'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_device_details 'AFC7: Eulerian 3-circle'
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '_w or _f'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK_a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            88560
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.01
_diffrn_source_current           200.0000
_diffrn_source_power             12.0000
_diffrn_source_voltage           60.0000
_exptl_absorpt_coefficient_mu    1.785
_exptl_absorpt_correction_T_max  0.6639
_exptl_absorpt_correction_T_min  0.5355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5112
_exptl_crystal_preparation
'mounted on a glass fiber with epoxy resin and placed in N2 stream at 153(2) K'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.179
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1570
_refine_ls_number_reflns         25831
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[_s^2^(Fo^2^)+(0.0503P)^2^+6.6714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                24566
_reflns_number_total             25831
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01833c.txt
_cod_data_source_block           NiBzBr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     'P 2ac 2ab '
_cod_original_sg_symbol_H-M      P212121
_cod_original_formula_sum        'C51.50 H60 Br2 N4 Ni O18'
_cod_database_code               7016025