Symmetric and non-symmetric bis-metallylene iron complexes, precursors of iron germanide nanoparticles
Sodreau, Alexandre; Lentz, Nicolas; Frutos, Maria; Ladeira, Sonia; Nayral, Celine; Delpech, Fabien; Madec, David; Chemical Communications  (2019) –; doi:10.1039/C9CC05063A

data_7123860
_publ_section_title
;
 Symmetric and non-symmetric bis-metallylene iron complexes, precursors of
 iron germanide nanoparticles
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05063A
_journal_year                    2019
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C44 H92 Cl4 N8 O2 Sn4'
_chemical_formula_sum            'C44 H92 Cl4 N8 O2 Sn4'
_chemical_formula_weight         1381.90
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2018-10-26 deposited with the CCDC.    2019-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.495(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9149(4)
_cell_length_b                   18.3126(8)
_cell_length_c                   16.2508(7)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      36.72
_cell_measurement_theta_min      3.54
_cell_volume                     2856.7(2)
_computing_cell_refinement       'APEX2 and SAINT'
_computing_data_collection       APEX2
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49041
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.142
_diffrn_reflns_theta_min         1.706
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.956
_exptl_absorpt_correction_T_max  0.7473
_exptl_absorpt_correction_T_min  0.6153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.569
_refine_diff_density_min         -1.882
_refine_diff_density_rms         0.502
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         10869
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.038
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0894P)^2^+1.3348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1522
_reflns_Friedel_coverage         0
_reflns_number_gt                8833
_reflns_number_total             10869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05063a2.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7123860
_shelx_res_checksum              65311