Isolation of chloride- and hydride-bridged tri-iron and -zinc clusters in a tris(β-oxo-δ-diimine) cyclophane ligand.
Hong, Dae Ho; Knight, Brian J.; Catalano, Vincent J.; Murray, Leslie J.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9570–9575; doi:10.1039/c9dt00799g

data_7049802
_publ_section_title
;
 Isolation of chloride- and hydride-bridged tri-iron and -zinc clusters in
 a tris(\b-oxo-\d-diimine) cyclophane ligand.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9570
_journal_page_last               9575
_journal_paper_doi               10.1039/c9dt00799g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C72 H90 Cl3 Fe3 N6 O3'
_chemical_formula_weight         1361.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-02-22 deposited with the CCDC.    2019-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.891(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9148(13)
_cell_length_b                   22.857(2)
_cell_length_c                   23.150(2)
_cell_measurement_reflns_used    4180
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.74
_cell_measurement_theta_min      2.37
_cell_volume                     6751.6(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1954
_diffrn_reflns_av_unetI/netI     0.1430
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            66004
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.259
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  .7451
_exptl_absorpt_correction_T_min  .5867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       rod
_exptl_crystal_F_000             2868
_exptl_crystal_size_max          0.469
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         11889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1764
_refine_ls_R_factor_gt           0.0829
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0695P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6322
_reflns_number_total             11889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00799g2.cif
_cod_data_source_block           lmdh04_0m
_cod_depositor_comments          'Adding full bibliography for 7049802.cif.'
_cod_original_cell_volume        6751.9(12)
_cod_database_code               7049802
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.704
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              81344