Crystal Structure of a Trigonally Compressed Hexakis-DMF Zinc(II) Complex
ITO, Misaki; MITSUHASHI, Ryoji; MIKURIYA, Masahiro; SAKIYAMA, Hiroshi; X-ray Structure Analysis Online 32 (2016) 21–; doi:10.2116/xraystruct.32.21

data_1551605
_publ_section_title
;
 Crystal Structure of a Trigonally Compressed Hexakis-DMF Zinc(II) Complex
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              21
_journal_paper_doi               10.2116/xraystruct.32.21
_journal_volume                  32
_journal_year                    2016
_chemical_formula_moiety         'C18 H42 N6 O6 Zn, 2(C24 H20 B)'
_chemical_formula_sum            'C66 H82 B2 N6 O6 Zn'
_chemical_formula_weight         1142.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   30.231(5)
_cell_length_b                   9.2503(14)
_cell_length_c                   22.083(3)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.893
_cell_measurement_theta_min      2.284
_cell_volume                     6175.4(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\p and \w'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37903
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.893
_diffrn_reflns_theta_min         2.284
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.299(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.634
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         14167
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.634
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0441P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.950
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.928
_reflns_number_gt                9848
_reflns_number_total             14167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            32_21_1.txt
_cod_data_source_block           ydkr_a
_cod_original_cell_volume        6175.2(16)
_cod_database_code               1551605
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.847
_shelx_estimated_absorpt_t_max   0.891
_shelx_res_checksum              59770
_shelx_hkl_checksum              80850