Diaqua(1,4,8,11-tetraazacyclotetradecane)nickel(II) fumarate tetrahydrate
Lim, Shao Liang; Ng, Chew Hee; Teoh, Siang Guan; Loh, Wan-Sin; Fun, Hoong-Kun; Acta Crystallographica Section E 66 (2010) m737–m738; doi:10.1107/S1600536810020064

data_2226698
_publ_section_title
;
 Diaqua(1,4,8,11-tetraazacyclotetradecane)nickel(II) fumarate
 tetrahydrate
;
_journal_coeditor_code           TK2677
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m737
_journal_page_last               m738
_journal_paper_doi               10.1107/S1600536810020064
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ni (C10 H24 N4) (H2 O)2] (C4 H2 O4), 4H2 O'
_chemical_formula_moiety         'C10 H28 N4 Ni O2 2+, C4 H2 O4 2-, 4(H2 O)'
_chemical_formula_sum            'C14 H38 N4 Ni O10'
_chemical_formula_weight         481.19
_chemical_name_common
;
Diaqua(1,4,8,11-tetraazacyclotetradecane)nickel(II) fumarate tetrahydrate
;
_chemical_name_systematic
;
Diaqua(1,4,8,11-tetraazacyclotetradecane)nickel(II) fumarate tetrahydrate
;
_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                73.165(2)
_cell_angle_beta                 79.207(2)
_cell_angle_gamma                85.227(2)
_cell_formula_units_Z            1
_cell_length_a                   6.9913(5)
_cell_length_b                   8.8313(7)
_cell_length_c                   9.3147(8)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      35.11
_cell_measurement_theta_min      3.75
_cell_volume                     540.47(7)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type
;
Bruker APEXII DUO CCD area-detector diffractometer
;
_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  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12800
_diffrn_reflns_theta_full        34.00
_diffrn_reflns_theta_max         34.00
_diffrn_reflns_theta_min         2.97
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  0.8054
_exptl_absorpt_correction_T_min  0.6652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             258
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.267
_refine_diff_density_min         -1.181
_refine_ls_extinction_coef       0.75(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.301
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         4295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.301
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max_lt       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^)+(0.0892P)^2^+0.0620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1333
_reflns_number_gt                4219
_reflns_number_total             4295
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2677.cif
_cod_data_source_block           I
_cod_database_code               2226698
_cod_database_fobs_code          2226698