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_7123862
_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 Si3'
_chemical_formula_sum            'C35 H64 Cl Fe Ge N5 O3 Si3'
_chemical_formula_weight         851.09
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 101.860(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.0059(14)
_cell_length_b                   9.9312(6)
_cell_length_c                   19.8961(13)
_cell_measurement_reflns_used    9250
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      37.15
_cell_measurement_theta_min      3.06
_cell_volume                     4448.7(5)
_computing_cell_refinement       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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            181117
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.031
_diffrn_reflns_theta_min         2.937
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.6779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         15462
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+3.7677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0
_reflns_number_gt                13332
_reflns_number_total             15462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05063a2.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7123862
_shelx_res_checksum              35715