(2-Carboxyacetato-κ^2^<i>O</i>^1^,<i>O</i>^1'^)(<i>rac</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 acetonitrile solvate
Ou, Guang-Chuan; Ng, Seik Weng; Acta Crystallographica Section E 66 (2010) m1468–; doi:10.1107/S1600536810042637

data_2227263
_publ_section_title
;
 (2-Carboxyacetato-\k^2^<i>O</i>^1^,<i>O</i>^1'^)(<i>rac</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 acetonitrile solvate
;
_journal_coeditor_code           BT5383
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1468
_journal_paper_doi               10.1107/S1600536810042637
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ni (C3 H3 O4) (C16 H36 N4)] Cl O4, C2 H3 N'
_chemical_formula_moiety         'C19 H39 N4 Ni O4 +, Cl O4 -, C2 H3 N'
_chemical_formula_sum            'C21 H42 Cl N5 Ni O8'
_chemical_formula_weight         586.76
_chemical_name_systematic
;
(2-Carboxyacetato-\k^2^<i>O</i>^1^,<i>O</i>^1'^)(<i>rac</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 acetonitrile solvate
;
_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                92.8990(10)
_cell_angle_beta                 107.3880(10)
_cell_angle_gamma                106.5160(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5236(4)
_cell_length_b                   10.1766(4)
_cell_length_c                   15.3372(6)
_cell_measurement_reflns_used    7463
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      2.3
_cell_volume                     1344.99(9)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker SMART APEX'
_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  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11181
_diffrn_reflns_theta_full        27.03
_diffrn_reflns_theta_max         27.03
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_T_max  0.8447
_exptl_absorpt_correction_T_min  0.6946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.544
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         5701
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.9446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0902
_reflns_number_gt                4946
_reflns_number_total             5701
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5383.cif
_cod_data_source_block           I
_cod_database_code               2227263
_cod_database_fobs_code          2227263