Diaqua[(1<i>R</i>,2<i>S</i>,4<i>R</i>,8<i>R</i>,9<i>S</i>,11<i>R</i>)-2,9-dimethyl-1,4,8,11-tetraazacyclotetradecane]nickel(II) dichloride dihydrate
Townsend, James Alan; Desper, John; Acta Crystallographica Section E 68 (2012) m1111–m1112; doi:10.1107/S160053681203276X

data_2235942
_publ_section_title
;
 Diaqua[(1<i>R</i>,2<i>S</i>,4<i>R</i>,8<i>R</i>,9<i>S</i>,11<i>R</i>)-2,9-dimethyl-1,4,8,11-tetraazacyclotetradecane]nickel(II)
 dichloride dihydrate
;
_journal_coeditor_code           PK2429
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1111
_journal_page_last               m1112
_journal_paper_doi               10.1107/S160053681203276X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ni (C12 H28 N4) (H2 O)2] Cl2, 2H2 O'
_chemical_formula_moiety         'C12 H32 N4 Ni O2 2+, 2(Cl -), 2(H2 O)'
_chemical_formula_sum            'C12 H36 Cl2 N4 Ni O4'
_chemical_formula_weight         430.06
_chemical_name_systematic
;
Diaqua[(1<i>R</i>,2<i>S</i>,4<i>R</i>,8<i>R</i>,9<i>S</i>,11<i>R</i>)-2,9-
dimethyl-1,4,8,11-tetraazacyclotetradecane]nickel(II) dichloride dihydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7309(8)
_cell_length_b                   14.0994(11)
_cell_length_c                   14.6000(11)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.24
_cell_measurement_theta_min      3.14
_cell_volume                     2003.1(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25180
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    1.257
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.384
_refine_ls_abs_structure_details 'Flack (1983), 3205 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.006(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         7454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0350P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                6563
_reflns_number_total             7454
_reflns_threshold_expression     I>\s(I)
_cod_data_source_file            pk2429.cif
_cod_data_source_block           I
_cod_database_code               2235942
_cod_database_fobs_code          2235942