<i>trans</i>-Aquachloro[(1<i>R</i>,4<i>R</i>,8<i>S</i>,11<i>S</i>)-6,13-diammonio-6,13-dimethyl-1,4,8,11-tetraazacyclotetradecane-κ^4^<i>N</i>^1,4,8,11^]nickel(II) trichloride trihydrate
Neil F. Curtis; Rebekah Pawley; Ward T. Robinson; Acta Crystallographica Section C 62 (2006) m352–m354; doi:10.1107/S0108270106010407

data_2015480
_publ_section_title
;<i>trans</i>-Aquachloro[(1<i>R</i>,4<i>R</i>,8<i>S</i>,11<i>S</i>)-6,13-diammonio-6,13-dimethyl-1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>^1,4,8,11^]nickel(II)
 trichloride trihydrate
;
_journal_coeditor_code           GA3002
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m352
_journal_page_last               m354
_journal_paper_doi               10.1107/S0108270106010407
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Ni Cl (C12 H32 N6) (H2 O)] Cl3, 3H2 O'
_chemical_formula_moiety         'C12 H34 Cl N6 Ni O 3+, 3Cl -, 3H2 O'
_chemical_formula_sum            'C12 H40 Cl4 N6 Ni O4'
_chemical_formula_weight         533.01
_chemical_name_systematic
;
trans-[Aqua-chloro-(1R,4R,8S,11S-trans-6,13-diazonium-6,13-dimethyl-
1,4,8,11-tetraazacyclortetradecane-\k^4^ N^1,4,8,11^)nickel(II)]
trichloride trihydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 103.6100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3750(10)
_cell_length_b                   10.5320(10)
_cell_length_c                   10.8930(10)
_cell_measurement_reflns_used    3552
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      3.11
_cell_volume                     1156.85(19)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'ORTEP3.2 (Farrugia, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0098
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3617
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.330
_exptl_absorpt_correction_T_max  0.653
_exptl_absorpt_correction_T_min  0.535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 1997)
;
_exptl_crystal_colour            blue--violet
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.311
_refine_ls_abs_structure_details 'Flack (1983), 313 Friedel pairs'
_refine_ls_abs_structure_Flack   0.012(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4243
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0167
_refine_ls_R_factor_gt           0.0164
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'calc w=1/[\s^2^(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0392
_refine_ls_wR_factor_ref         0.0395
_reflns_number_gt                3243
_reflns_number_total             3315
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ga3002.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_angle_publ_flag' value 'N' changed to 'n' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (2 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_angle_publ_flag' value 'N' changed to 'n' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (2 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1156.9(2)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2015480
_cod_database_fobs_code          2015480