Crystal structures of two nickel(II) macrocyclic salts: (5,7,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II) bis(perchlorate) monohydrate and (5,7,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II) dibromide trihydrate
Corfield, Peter W. R.; Goedken, Virgil L.; Acta Crystallographica Section E 75 (2019) 332–337; doi:10.1107/S2056989019002056

data_2242849
_publ_section_title
;
 Crystal structures of two nickel(II) macrocyclic salts:
 (5,7,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II)
 bis(perchlorate) monohydrate and
 (5,7,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II)
 dibromide trihydrate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              332
_journal_page_last               337
_journal_paper_doi               10.1107/S2056989019002056
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Ni (C16 H36 N4)] Br2, 3H2 O'
_chemical_formula_moiety         'C16 H36 N4 Ni 2+, 2(Br -), 3(H2 O)'
_chemical_formula_sum            'C16 H42 Br2 N4 Ni O3'
_chemical_formula_weight         557.06
_chemical_name_systematic
;
(5,7,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II)
dibromide trihydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   60.3649(18)
_cell_length_b                   19.8364(9)
_cell_length_c                   7.9773(3)
_cell_measurement_reflns_used    6096
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.41
_cell_volume                     9552.2(6)
_computing_cell_refinement
;
SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
KappaCCD Server Software (Nonius, 1997)
;
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia,
2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
Corfield & Gainsford (1972)
;
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Enraf--Nonius KappaCCD'
_diffrn_measurement_method       'combination of \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.096
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_limit_h_max       78
_diffrn_reflns_limit_h_min       -78
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            41142
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         2.161
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.170
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.34
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(SCALEPACK; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_meas      1.530(3)
_exptl_crystal_density_method
'Flotation in chloroform/carbon tetrachloride mixtures'
_exptl_crystal_description       rod
_exptl_crystal_F_000             4608
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.557
_refine_ls_abs_structure_details
;
Twinning involves inversion,with Flack parameter corresponding to twin-fraction
occupancies
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5382
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+35.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                4897
_reflns_number_total             5382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2613sup1.cif
_cod_data_source_block           II
_cod_database_code               2242849
_shelx_estimated_absorpt_t_min   0.307
_shelx_estimated_absorpt_t_max   0.680
_shelx_hkl_checksum              55918
_shelx_res_checksum              17527
_cod_database_fobs_code 2242849