Acetate and acetamide complexes of [Ni(Me~4~[12]aneN~4~)]PF~6~: a tale of two ligands
Wallick, Jessica L.; Riordan, Charles G.; Yap, Glenn P. A.; Acta Crystallographica Section C 70 (2014) 640–643; doi:10.1107/S2053229614011620

data_2019580
_publ_section_title
;
 Acetate and acetamide complexes of [Ni(Me~4~[12]aneN~4~)]PF~6~: a tale of
 two ligands
;
_journal_coeditor_code           SF3230
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              640
_journal_page_last               643
_journal_paper_doi               10.1107/S2053229614011620
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Ni (C2 H3 O2) (C12 H28 N4)] P F6'
_chemical_formula_moiety         'C14 H31 N4 Ni O2 +, F6 P1 -'
_chemical_formula_sum            'C14 H31 F6 N4 Ni O2 P'
_chemical_formula_weight         491.11
_chemical_name_systematic
'(Acetato-\k^2^<i>O</i>,<i>O</i>')(1,4,7,10-tetramethyl-1,4,7,10-tetraazacyclododecane-\k^4^<i>N</i>)nickel(II) hexafluoridophosphate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 99.929(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5588(10)
_cell_length_b                   11.7643(11)
_cell_length_c                   17.2263(16)
_cell_measurement_reflns_used    2513
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20.88
_cell_measurement_theta_min      2.40
_cell_volume                     2107.7(3)
_computing_cell_refinement       'APEX2 (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'APEX2 (Bruker, 2007)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11775
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.701
_diffrn_reflns_theta_min         2.401
_exptl_absorpt_coefficient_mu    1.065
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       needle
_exptl_crystal_F_000             1024
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_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.120
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_refine_diff_density_min         -0.303
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.143(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4725
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0446P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                4117
_reflns_number_total             4725
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3230sup1.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 2019580--2019581.cif.'
_cod_database_code               2019580
_cod_database_fobs_code          2019580
_shelx_estimated_absorpt_t_min   0.818
_shelx_estimated_absorpt_t_max   0.883
_shelx_hkl_checksum              40476
_shelx_res_checksum              12339
_shelxl_version_number           .2013