Preorganized assembly of three iron(II) or manganese(II) beta-diketiminate complexes using a cyclophane ligand
Gary L. Guillet; Forrest T. Sloane; David M. Ermert; Matthew W. Calkins; Marcus K. Peprah; Elisabeth S. Knowles; Erik Cizmar; Khalil A. Abboud; Mark W. Meisel; Leslie J. Murray; Chem.Commun. 49 (2013) 6635–; doi:10.1039/c3cc43395a

data_7109517
_publ_section_title
;
 Preorganized assembly of three iron(II) or manganese(II)
 beta-diketiminate complexes using a cyclophane ligand
;
_journal_name_full               Chem.Commun.
_journal_page_first              6635
_journal_paper_doi               10.1039/c3cc43395a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C52 H71 Br3 Fe3 N6, 2(C7 H8)'
_chemical_formula_sum            'C66 H87 Br3 Fe3 N6'
_chemical_formula_weight         1371.70
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_audit_update_record
;
2012-12-18 # Formatted by publCIF
;
_cell_angle_alpha                90.828(2)
_cell_angle_beta                 96.343(2)
_cell_angle_gamma                102.824(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8711(12)
_cell_length_b                   15.8346(16)
_cell_length_c                   16.9540(17)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      2.22
_cell_volume                     3085.9(5)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Triumph'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52627
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.75
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.683
_exptl_absorpt_correction_T_max  0.8001
_exptl_absorpt_correction_T_min  0.6132
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL v6.14 (Bruker 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.969
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         14157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0363P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0710
_reflns_number_gt                10123
_reflns_number_total             14157
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3cc43395a.txt
_cod_data_source_block           ylee37
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7109517