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_7123861
_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_formula_moiety         'C35 H64 Cl Fe Ge N5 O3 Si2 Sn'
_chemical_formula_sum            'C35 H64 Cl Fe Ge N5 O3 Si2 Sn'
_chemical_formula_weight         941.71
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 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                 105.207(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8967(4)
_cell_length_b                   33.0836(13)
_cell_length_c                   13.0091(6)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      3.09
_cell_volume                     4525.6(3)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.037
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38811
_diffrn_reflns_point_group_measured_fraction_full 0.825
_diffrn_reflns_point_group_measured_fraction_max 0.825
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.481
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.672
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.876
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 3926 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1022
_refine_ls_number_reflns         14165
_refine_ls_number_restraints     260
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+1.5761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.653
_reflns_Friedel_fraction_full    0.654
_reflns_Friedel_fraction_max     0.653
_reflns_number_gt                11897
_reflns_number_total             14165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05063a2.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               7123861
_shelx_res_checksum              42898