5-Ferrocenylmethyl-2,2-dimethyl-5-(prop-2-ynyl)-1,3-dioxane-4,6-dione
Naier, Benjamin; Laus, Gerhard; Wurst, Klaus; Schottenberger, Herwig; IUCrData 1 (2016) x160569–; doi:10.1107/S2414314616005691

data_1543084
_publ_section_title
;
 5-Ferrocenylmethyl-2,2-dimethyl-5-(prop-2-ynyl)-1,3-dioxane-4,6-dione
;
_journal_coeditor_code           WM4012
_journal_issue                   4
_journal_name_full               IUCrData
_journal_page_first              x160569
_journal_paper_doi               10.1107/S2414314616005691
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          '[Fe (C5 H5) (C15 H15 O4)]'
_chemical_formula_moiety         'C20 H20 Fe O4'
_chemical_formula_sum            'C20 H20 Fe O4'
_chemical_formula_weight         380.21
_chemical_name_systematic
;
5-Ferrocenylmethyl-2,2-dimethyl-5-(prop-2-ynyl)-1,3-dioxane-4,6-dione
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.9560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8263(4)
_cell_length_b                   7.4617(2)
_cell_length_c                   11.9888(4)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      50.6
_cell_measurement_theta_min      5.2
_cell_volume                     878.52(5)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.450
_diffrn_reflns_theta_min         2.636
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2012)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       plate
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.165
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1346 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.009(6)
_refine_ls_extinction_coef       0.019(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015<i>b</i>)
;
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3215
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0212
_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^)+(0.0281P)^2^+0.1144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0521
_reflns_number_gt                3078
_reflns_number_total             3215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4012sup1.cif
_cod_data_source_block           I
_cod_database_code               1543084
_shelx_estimated_absorpt_t_min   0.858
_shelx_estimated_absorpt_t_max   0.941
_shelx_hkl_checksum              70968
_shelx_res_checksum              82113
_cod_database_fobs_code 1543084