4-Methyl-2,7-dioxo-3,6-dioxa-1(1,1')-ferrocenacycloheptaphane
Leng, Xin; Yang, Bingqin; Zhang, Pengfei; Fang, Xianwen; Acta Crystallographica Section E 67 (2011) m947–; doi:10.1107/S1600536811019398

data_2230705
_publ_section_title
;
 4-Methyl-2,7-dioxo-3,6-dioxa-1(1,1')-ferrocenacycloheptaphane
;
_journal_coeditor_code           HY2432
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m947
_journal_paper_doi               10.1107/S1600536811019398
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Fe (C15 H14 O4)]'
_chemical_formula_moiety         'C15 H14 Fe O4'
_chemical_formula_sum            'C15 H14 Fe O4'
_chemical_formula_weight         314.11
_chemical_melting_point          405(6)
_chemical_name_common
;
4-Methyl-2,7-dioxo-3,6-dioxa-1(1,1')-ferrocenacycloheptaphane
;
_chemical_name_systematic
;
propane-1,2-diyl ferrocene-1,1'-dicarboxylate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.193(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1665(14)
_cell_length_b                   20.131(4)
_cell_length_c                   9.2464(19)
_cell_measurement_temperature    296(2)
_cell_volume                     1298.8(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3177
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_T_max  0.8703
_exptl_absorpt_correction_T_min  0.7269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.405
_refine_ls_abs_structure_details 'Flack (1983), 812 Friedel pairs'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1971
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0495P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                1721
_reflns_number_total             1971
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2432.cif
_cod_data_source_block           I
_cod_original_cell_volume        1298.7(4)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2230705
_cod_database_fobs_code          2230705