Crystal structure of bis{5-(N,N′-diethylamine)-5′-methoxy -2,2′-[ethylenediyldioxybis(nitrilomethylidyne)]diphenolato}-bis(μ2-acetato-κ2 O:O′)trizinc(II), C46H56Zn3N6O14
Dong, Xiu-Yan; Zhang, Han; Wang, Bai-Jun; Lan, Peng-Fei; Dong, Wen-Kui; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 881–883; doi:10.1515/ncrs-2017-0038

data_8106708
_publ_section_title
;
 Crystal structure of bis{5-(N,N&#x2032;-diethylamine)-5&#x2032;-methoxy
 -2,2&#x2032;-[ethylenediyldioxybis(nitrilomethylidyne)]diphenolato}-bis(\m2-acetato-\k2
 O:O&#x2032;)trizinc(II), C46H56Zn3N6O14
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              881
_journal_page_last               883
_journal_paper_doi               10.1515/ncrs-2017-0038
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C46 H56 N6 O14 Zn3'
_chemical_formula_sum            'C46 H56 N6 O14 Zn3'
_chemical_formula_weight         1113.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.246(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6703(7)
_cell_length_b                   27.091(4)
_cell_length_c                   17.9132(16)
_cell_measurement_reflns_used    1437
_cell_measurement_temperature    290.92(10)
_cell_measurement_theta_max      22.2670
_cell_measurement_theta_min      3.7730
_cell_volume                     5147.4(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      290.92(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -20.00   23.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3571  -99.0000  -90.0000 43

  2 omega   38.00   94.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946  178.0000  -60.0000 56

  3 omega   -3.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946   38.0000  150.0000 93

  4 omega    4.00   40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946  -57.0000    0.0000 36
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0272629000
_diffrn_orient_matrix_UB_12      -0.0220178000
_diffrn_orient_matrix_UB_13      0.0158819000
_diffrn_orient_matrix_UB_21      0.0511300000
_diffrn_orient_matrix_UB_22      0.0138272000
_diffrn_orient_matrix_UB_23      0.0179724000
_diffrn_orient_matrix_UB_31      -0.0333524000
_diffrn_orient_matrix_UB_32      0.0031829000
_diffrn_orient_matrix_UB_33      0.0317947000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_unetI/netI     0.1118
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10608
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.61
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1324
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+1.2018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1865
_reflns_number_gt                2787
_reflns_number_total             5060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2017-0038_suppl.cif
_cod_data_source_block           d568
_cod_original_cell_volume        5147.4(9)
_cod_database_code               8106708