<i>trans</i>-Dioxocyclam (1,4,8,11-tetraazacyclotetradecane-2,9-dione) dihydrate and its Ni^II^ complex
Hubin, Timothy J.; Tyryshkin, Nickolay; Alcock, Nathaniel W.; Busch, Daryle H.; Acta Crystallographica Section C 57 (2001) 359–362; doi:10.1107/S0108270100020308

data_2011853
_publ_section_title
;
 <i>trans</i>-Dioxocyclam (1,4,8,11-tetraazacyclotetradecane-2,9-dione)
 dihydrate and its Ni^II^ complex
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              359
_journal_page_last               362
_journal_paper_doi               10.1107/S0108270100020308
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[Ni (C10 H18 N4 O2)] , 2H2 O'
_chemical_formula_moiety         'C10 H18 N4 Ni O2 , 2H2 O'
_chemical_formula_sum            'C10 H22 N4 Ni O4'
_chemical_formula_weight         321.03
_chemical_name_systematic
;
(1,4,8,11-tetraazacyclotetradecane-2,9-dione-\k^4^N)nickel(II) dihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 112.205(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.861(3)
_cell_length_b                   7.3385(10)
_cell_length_c                   9.6130(13)
_cell_measurement_reflns_used    1275
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     1362.5(3)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full .996
_diffrn_measured_fraction_theta_max .996
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .073
_diffrn_reflns_av_sigmaI/netI    .095
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3255
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.441
_exptl_absorpt_correction_T_max  .96
_exptl_absorpt_correction_T_min  .67
_exptl_absorpt_correction_type   \y-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             680
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .04
_refine_diff_density_max         .90
_refine_diff_density_min         -.53
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          .107
_refine_ls_R_factor_gt           .060
_refine_ls_shift/su_max          .025
_refine_ls_shift/su_mean         .002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.079P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .153
_reflns_number_gt                799
_reflns_number_total             1193
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm1440.cif
_cod_data_source_block           II
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2018-02-05

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_enum 1527 2010-12-29 10:47:43Z saulius 

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      'C 2/c'
_cod_database_code               2011853
_cod_database_fobs_code          2011853