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_2242848
_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_coeditor_code           PK2613
_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)]2 (Cl O4)4, H2 O'
_chemical_formula_moiety         '2(C16 H36 N4 Ni 2+), 4(Cl O4 -), H2 O'
_chemical_formula_sum            'C32 H74 Cl4 N8 Ni2 O17'
_chemical_formula_weight         1102.21
_chemical_name_systematic
;
(5,7,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II)
bis(perchlorate) hemihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 107.030(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.906(4)
_cell_length_b                   29.412(11)
_cell_length_c                   19.505(9)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      5.2
_cell_volume                     4885(4)
_computing_cell_refinement
;
Corfield & Gainsford (1972)
;
_computing_data_collection
;
Corfield & Gainsford (1972)
;
_computing_data_reduction
;
Data reduction followed procedures in Corfield <i>et al.</i> (1973) with
p = 0.05
;
_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
;
heavy atom method with local programs
;
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Picker 4-circle'
_diffrn_measurement_method       '\q/2\q scans'
_diffrn_radiation_monochromator  'oriented graphite 200 reflection'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7450
_diffrn_reflns_theta_full        58.381
_diffrn_reflns_theta_max         58.381
_diffrn_reflns_theta_min         2.806
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_decay_%        2(5)
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.599
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.454
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(Busing & Levy, 1957)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_meas      1.49
_exptl_crystal_density_method
'flotation in chloroform/carbon tetrachloride mixtures'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          .52
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .11
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.305
_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     686
_refine_ls_number_reflns         6870
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.04341
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                4899
_reflns_number_total             6870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2613sup1.cif
_cod_data_source_block           I
_cod_database_code               2242848
_cod_database_fobs_code          2242848
_shelx_estimated_absorpt_t_min   0.256
_shelx_estimated_absorpt_t_max   0.693
_shelx_hkl_checksum              59722
_shelx_res_checksum              98858