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_4126359
_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         'C62 H76 B2 Fe N10 O6, 2(H2 O)'
_chemical_formula_sum            'C62 H80 B2 Fe N10 O8'
_chemical_formula_weight         1170.83
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                100.432(3)
_cell_angle_beta                 104.367(3)
_cell_angle_gamma                92.736(2)
_cell_formula_units_Z            2
_cell_length_a                   14.5285(4)
_cell_length_b                   14.8368(4)
_cell_length_c                   14.9997(5)
_cell_measurement_reflns_used    7973
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.3340
_cell_measurement_theta_min      4.1440
_cell_volume                     3065.79(17)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1333
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.959
_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   -116.00 -23.00   1.00    7.50    --  -41.76 -37.00  60.00   93
  2  \w    -85.00  -8.00   1.00    7.50    --  -41.76 125.00-150.00   77
  3  \w    -67.00  27.00   1.00    7.50    --  -41.76  57.00-150.00   94
  4  \w     63.00  90.00   1.00    7.50    --   41.76-125.00-150.00   27
  5  \w      9.00  92.00   1.00    7.50    --   41.76  77.00  30.00   83
  6  \w     18.00  80.00   1.00    7.50    --   41.76  19.00  30.00   62
  7  \w     38.00 139.00   1.00   30.00    --  110.51 -61.00  60.00  101
  8  \w     39.00 114.00   1.00   30.00    --  110.51 -61.00-180.00   75
  9  \w     32.00 158.00   1.00   30.00    --  110.51 -15.00 120.00  126
 10  \w     80.00 121.00   1.00   30.00    --  110.51-125.00 -30.00   41
 11  \w     40.00  66.00   1.00   30.00    --  110.51-125.00 -30.00   26
 12  \w     36.00 136.00   1.00   30.00    --  110.51 -30.00 -60.00  100
 13  \w     69.00 103.00   1.00   30.00    --  110.51 -94.00-180.00   34
 14  \w     93.00 178.00   1.00   30.00    --  110.51  45.00 120.00   85
 15  \w     78.00 120.00   1.00   30.00    --  110.51-125.00 150.00   42
 16  \w     97.00 143.00   1.00   30.00    --  110.51  45.00 150.00   46
 17  \w     34.00 135.00   1.00   30.00    --  110.51 -77.00 -60.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_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  0.0441
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21172
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.865
_diffrn_reflns_theta_min         3.155
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.471
_exptl_absorpt_correction_T_max  0.767
_exptl_absorpt_correction_T_min  0.491
_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            'clear light orange'
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       plate
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     828
_refine_ls_number_reflns         12259
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0877P)^2^+0.5676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10470
_reflns_number_total             12259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b04861_si_013.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        3065.77(17)
_cod_database_code               4126359
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              38519
_shelx_hkl_checksum              24070
_shelx_fab_checksum              92621