(Cinnamato-κ^2^<i>O</i>,<i>O</i>')(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ^4^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''')nickel(II) perchlorate monohydrate
Gao, Qiang; Cao, Yi-Cheng; Acta Crystallographica Section E 68 (2012) m1100–; doi:10.1107/S1600536812032175

data_2235780
_publ_section_title
;
 (Cinnamato-\k^2^<i>O</i>,<i>O</i>')(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''')nickel(II)
 perchlorate monohydrate
;
_journal_coeditor_code           DS2203
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1100
_journal_paper_doi               10.1107/S1600536812032175
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ni (C9 H7 O2) (C16 H36 N4)] Cl O4, H2 O'
_chemical_formula_moiety         'C25 H43 N4 Ni O2 +, Cl O4 -, H2 O'
_chemical_formula_sum            'C25 H45 Cl N4 Ni O7'
_chemical_formula_weight         607.81
_chemical_name_systematic
;
(Cinnamato-\k^2^<i>O</i>,<i>O</i>')(5,5,7,12,12,14-hexamethyl-1,4,8,11-
tetraazacyclotetradecane-
\k^4^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''')nickel(II) perchlorate
monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.225(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6903(11)
_cell_length_b                   14.5396(8)
_cell_length_c                   19.2498(12)
_cell_measurement_reflns_used    10750
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      65.54
_cell_measurement_theta_min      3.81
_cell_volume                     2983.9(4)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2011)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2011)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2011)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Agilent Xcalibur Atlas Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10750
_diffrn_reflns_theta_full        65.54
_diffrn_reflns_theta_max         65.54
_diffrn_reflns_theta_min         3.81
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.158
_exptl_absorpt_correction_T_max  0.7240
_exptl_absorpt_correction_T_min  0.4643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2011)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.534
_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     355
_refine_ls_number_reflns         5001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0494P)^2^+2.0261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                4533
_reflns_number_total             5001
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ds2203.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2235780
_cod_database_fobs_code          2235780