(5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene-κ^4^<i>N</i>^1^,<i>N</i>^4^,<i>N</i>^8^,<i>N</i>^11^)(thiocyanato-κ<i>S</i>)nickel(II) perchlorate monohydrate
Bi, Jian-Hong; Acta Crystallographica Section E 65 (2009) m668–; doi:10.1107/S1600536809018091

data_2221987
_publ_section_title
;(5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene-\k^4^<i>N</i>^1^,<i>N</i>^4^,<i>N</i>^8^,<i>N</i>^11^)(thiocyanato-\k<i>S</i>)nickel(II)
 perchlorate monohydrate
;
_journal_coeditor_code           CV2562
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m668
_journal_paper_doi               10.1107/S1600536809018091
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni (N C S) (C16 H32 N4)] Cl O4, H2 O'
_chemical_formula_moiety         'C17 H32 N5 Ni S +, Cl O4 -, H2 O'
_chemical_formula_sum            'C17 H34 Cl N5 Ni O5 S'
_chemical_formula_weight         514.71
_chemical_name_systematic
;
(5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene-
\k^4^<i>N</i>^1^,<i>N</i>^4^,<i>N</i>^8^,<i>N</i>^11^)(thiocyanato-
\kS)nickel(II) perchlorate monohydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.1430(10)
_cell_angle_beta                 87.005(2)
_cell_angle_gamma                67.3480(10)
_cell_formula_units_Z            2
_cell_length_a                   7.2678(11)
_cell_length_b                   8.9998(13)
_cell_length_c                   19.513(2)
_cell_measurement_reflns_used    2923
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.666
_cell_measurement_theta_min      2.462
_cell_volume                     1171.6(3)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6103
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    1.068
_exptl_absorpt_correction_T_max  0.6808
_exptl_absorpt_correction_T_min  0.6226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.895
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0501P)^2^+0.9082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1087
_reflns_number_gt                3247
_reflns_number_total             4062
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv2562.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Triclinic' changed to 'triclinic'
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_database_code               2221987
_cod_database_fobs_code          2221987