[3]Ferrocenophanes with the bisphosphanotetryl bridge: inorganic rings on the way to tetrylenes.
Kargin, Denis; Kelemen, Zsolt; Krekić, Kristijan; Maurer, Martin; Bruhn, Clemens; Nyulászi, László; Pietschnig, Rudolf; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2180–2189; doi:10.1039/c5dt03107a

data_7038169
_publ_section_title
;
 [3]Ferrocenophanes with the bisphosphanotetryl bridge: inorganic rings on
 the way to tetrylenes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2180
_journal_page_last               2189
_journal_paper_doi               10.1039/c5dt03107a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C24 H44 Fe P2 Si2'
_chemical_formula_weight         506.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-10-30 deposited with the CCDC.
2015-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9505(7)
_cell_length_b                   9.6294(9)
_cell_length_c                   31.735(3)
_cell_measurement_reflns_used    35563
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.13
_cell_measurement_theta_min      2.21
_cell_volume                     2735.2(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      ' 1124 frames, detector distance = 80 mm'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            30487
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.210
_diffrn_source                   'Mo Genix'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  0.9519
_exptl_absorpt_correction_T_min  0.8579
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-red ver. 1.58 (Stoe & Cie. 2012)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       plate
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 2151 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0324P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0598
_reflns_Friedel_coverage         0.748
_reflns_friedel_fraction_full    0.988
_reflns_friedel_fraction_max     0.990
_reflns_number_gt                5356
_reflns_number_total             5940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03107a3.cif
_cod_data_source_block           sv0106
_cod_database_code               7038169
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.781
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              42828
_shelx_hkl_checksum              7219