Crystal Structure of Bis(acetone-<i>&kappa;</i><i>O</i>)-1,4,8,11-tetraazacyclotetradecane Copper(II) Ditetraphenylborate Acetone Disolvate
MATSUI, Chihiro; OKAWARA, Toru; NAGAMURA, Toshihiko; TAKEHARA, Kenji; X-ray Structure Analysis Online 31 (2015) 53–; doi:10.2116/xraystruct.31.53

data_1551641
_publ_section_title
;
 Crystal Structure of
 Bis(acetone-&lt;i&gt;&amp;kappa;&lt;/i&gt;&lt;i&gt;O&lt;/i&gt;)-1,4,8,11-tetraazacyclotetradecane
 Copper(II) Ditetraphenylborate Acetone Disolvate
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              53
_journal_paper_doi               10.2116/xraystruct.31.53
_journal_volume                  31
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety
;
C16 H36 Cu N4 O2, 2(C24 H20 B), 2(C3 H6 O)
;
_chemical_formula_sum            'C70 H88 B2 Cu N4 O4'
_chemical_formula_weight         1134.60
_chemical_name_systematic
;
Bis(acetone-\kO)-1,4,8,11-tetraazacyclotetradecane Copper(II) 
Ditetraphenylborate Acetone Disolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                100.526(2)
_cell_angle_beta                 107.4237(19)
_cell_angle_gamma                116.1558(19)
_cell_formula_units_Z            1
_cell_length_a                   12.2123(15)
_cell_length_b                   12.5684(16)
_cell_length_c                   12.9841(16)
_cell_measurement_reflns_used    4356
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.8283
_cell_measurement_theta_min      2.7426
_cell_volume                     1587.4(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker SMART APEX2'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'ORTEP3 for Windows'
_computing_publication_material  enCIFer
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SMART APEX2'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11074
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.77
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             607
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.601
_refine_ls_abs_structure_details 'Refined as an inversion twin.'
_refine_ls_abs_structure_Flack   0.17(3)
_refine_ls_extinction_coef       0.0066(10)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     792
_refine_ls_number_reflns         9103
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.5348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                7862
_reflns_number_total             9103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            31_53_1.txt
_cod_data_source_block           I
_cod_database_code               1551641