Photocrystallographic identification of metastable nitrito linkage isomers in a series of nickel(II) complexes.
Brayshaw, Simon K.; Easun, Timothy L.; George, Michael W.; Griffin, Alexandra M. E.; Johnson, Andrew L.; Raithby, Paul R.; Savarese, Teresa L.; Schiffers, Stefanie; Warren, John E.; Warren, Mark R.; Teat, Simon J.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 90–97; doi:10.1039/c1dt11379h

data_7017729
_publ_section_title
;
 Photocrystallographic identification of metastable nitrito linkage
 isomers in a series of nickel(II) complexes.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              90
_journal_page_last               97
_journal_paper_doi               10.1039/c1dt11379h
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C14 H32 N6 Ni O4'
_chemical_formula_sum            'C14 H32 N6 Ni O4'
_chemical_formula_weight         407.17
_chemical_name_systematic
;
Trans-bis[1-(2-amino-ethyl)-piperidine]dinitro-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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.03(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.629(5)
_cell_length_b                   8.240(2)
_cell_length_c                   11.804(2)
_cell_measurement_reflns_used    5420
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      66.868
_cell_measurement_theta_min      7.244
_cell_volume                     885.4(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    POVRAY
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTS (Sheldrick, 1997)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_measurement_method       '3000 0.3 degree images with \f and \w scans'
_diffrn_radiation_monochromator  'Channel-cut Si(111)'
_diffrn_radiation_source         'Station 11.3.1 ALS'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8704
_diffrn_reflns_theta_full        33.56
_diffrn_reflns_theta_max         33.56
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    1.422
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.767324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS - Bruker2004'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2605
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                2274
_reflns_number_total             2605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11379h.txt
_cod_data_source_block           1
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7017729