Design, Synthesis, and Structural Characterization of a New Class of Ferrocene-Containing Heterometallic Triple-Stranded Helicates
Raja, Muthukrishna; Iyer, Ratnasabapathy G.; Gwengo, Chengeto; Reger, Daniel L.; Pellechia, Perry J.; Smith, Mark D.; Pascui, Andrea E.; Organometallics 32 (2013) 95–; doi:10.1021/om300843r

data_4079803
_publ_section_title
;
 Design, Synthesis, and Structural Characterization of a New Class of
 Ferrocene-Containing Heterometallic Triple-Stranded Helicates
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              95
_journal_paper_doi               10.1021/om300843r
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         '0.25(C124 H100 Fe8 N4 O16), 0.06(C4 H8 Cl8)'
_chemical_formula_sum            'C31.25 H25.5 Cl0.5 Fe2 N O4'
_chemical_formula_weight         608.45
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           77
_space_group_name_Hall           'P 4c'
_space_group_name_H-M_alt        'P 42'
_symmetry_space_group_name_Hall  'P 4c'
_symmetry_space_group_name_H-M   'P 42'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-08-28
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.741(2)
_cell_length_b                   29.741(2)
_cell_length_c                   5.8917(5)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.83
_cell_measurement_theta_min      2.264
_cell_volume                     5211.4(7)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            8024
_diffrn_reflns_theta_full        43.87
_diffrn_reflns_theta_max         43.87
_diffrn_reflns_theta_min         1.49
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    9.723
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2500
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.038(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         2765
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+15.4698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1425
_reflns_number_gt                2243
_reflns_number_total             2765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300843r_si_001.cif
_cod_data_source_block           cg
_cod_original_formula_sum        'C31.25 H25.50 Cl0.50 Fe2 N O4'
_cod_database_code               4079803