The Intricate Structural Chemistry of M(II)2nLn-Type Assemblies.
Cecot, Giacomo; Marmier, Mathieu; Geremia, Silvano; De Zorzi, Rita; Vologzhanina, Anna V.; Pattison, Philip; Solari, Euro; Fadaei Tirani, Farzaneh; Scopelliti, Rosario; Severin, Kay; Journal of the American Chemical Society 139 (2017) 8371–8381; doi:10.1021/jacs.7b04861

data_4126362
_publ_section_title
;
 The Intricate Structural Chemistry of M(II)2nLn-Type Assemblies.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8371
_journal_page_last               8381
_journal_paper_doi               10.1021/jacs.7b04861
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         '2(C68 H61 B2 N10 O9 Zn2), C8 H20 N'
_chemical_formula_sum            'C144 H142 B4 N21 O18 Zn4'
_chemical_formula_weight         2759.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                69.7864(11)
_cell_angle_beta                 70.5451(11)
_cell_angle_gamma                88.8770(9)
_cell_formula_units_Z            4
_cell_length_a                   22.9158(3)
_cell_length_b                   23.8401(3)
_cell_length_c                   34.0163(4)
_cell_measurement_reflns_used    63409
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      76.2240
_cell_measurement_theta_min      3.9840
_cell_volume                     16347.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -69.00  32.00   1.00    2.00    --  -40.91  57.00-150.00  101
  2  \w    -94.00  -2.00   1.00    2.00    --  -40.91 125.00-120.00   92
  3  \w     49.00  97.00   1.00    2.00    --   40.91-125.00  60.00   48
  4  \w     58.00 111.00   1.00    8.00    --  112.00-111.00  90.00   53
  5  \w    111.00 144.00   1.00    8.00    --  112.00 -77.00 150.00   33
  6  \w     90.00 142.00   1.00    8.00    --  112.00 -77.00  30.00   52
  7  \w    103.00 130.00   1.00    8.00    --  112.00 -30.00 -60.00   27
  8  \w     84.00 176.00   1.00    8.00    --  112.00  30.00-120.00   92
  9  \w    103.00 147.00   1.00    8.00    --  112.00  61.00 -90.00   44
 10  \w     99.00 141.00   1.00    8.00    --  112.00  61.00  30.00   42
 11  \w    147.00 175.00   1.00    8.00    --  112.00  30.00 120.00   28
 12  \w     84.00 154.00   1.00    8.00    --  112.00  61.00 120.00   70
 13  \w     87.00 140.00   1.00    8.00    --  112.00  30.00 120.00   53
 14  \w     84.00 177.00   1.00    8.00    --  112.00  61.00 150.00   93
 15  \w    112.00 151.00   1.00    8.00    --  112.00 178.00  30.00   39
 16  \w     70.00  95.00   1.00    8.00    --  112.00 178.00  30.00   25
 17  \w     65.00 116.00   1.00    8.00    --  112.00 178.00 -60.00   51
 18  \w     84.00 142.00   1.00    8.00    --  112.00  61.00-180.00   58
 19  \w     84.00 134.00   1.00    8.00    --  112.00  15.00 -60.00   50
 20  \w     71.00 108.00   1.00    8.00    --  112.00 -94.00   0.00   37
 21  \w     80.00 113.00   1.00    8.00    --  112.00-111.00 -30.00   33
 22  \w     69.00 116.00   1.00    8.00    --  112.00-111.00-120.00   47
 23  \w     59.00 116.00   1.00    8.00    --  112.00-111.00-150.00   57
 24  \w     39.00 138.00   1.00    8.00    --  112.00 -45.00-180.00   99
 25  \w     41.00 136.00   1.00    8.00    --  112.00 -61.00 -30.00   95
 26  \w     89.00 114.00   1.00    8.00    --  112.00-111.00 150.00   25
 27  \w     41.00  66.00   1.00    8.00    --  112.00 -77.00  30.00   25
 28  \w     37.00 116.00   1.00    8.00    --  112.00-111.00   0.00   79
 29  \w     37.00  62.00   1.00    8.00    --  112.00 -77.00 150.00   25
 30  \w     36.00  62.00   1.00    8.00    --  112.00 -30.00 -60.00   26
 31  \w   -107.00 -20.00   1.00    2.00    --  -40.91 -38.00 -30.00   87
 32  \w   -115.00 -16.00   1.00    2.00    --  -40.91 -38.00  60.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            176555
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.935
_diffrn_reflns_theta_min         3.709
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.162
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_description       prism
_exptl_crystal_F_000             5748
_exptl_crystal_size_max          0.547
_exptl_crystal_size_mid          0.313
_exptl_crystal_size_min          0.271
_refine_diff_density_max         1.350
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3459
_refine_ls_number_reflns         67480
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+15.8895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                57662
_reflns_number_total             67480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b04861_si_015.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        16347.4(4)
_cod_database_code               4126362
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              25393
_shelx_hkl_checksum              94817
_shelx_fab_checksum              74915