Concise access to iminophosphonamide stabilized heteroleptic germylenes: chemical reactivity and structural investigation.
Prashanth, Billa; Singh, Sanjay; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6079–6087; doi:10.1039/c5dt02287h

data_7036717
_publ_section_title
;
 Concise access to iminophosphonamide stabilized heteroleptic germylenes:
 chemical reactivity and structural investigation.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6079
_journal_page_last               6087
_journal_paper_doi               10.1039/c5dt02287h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C32 H36 Cl Fe Ge N2 O4 P'
_chemical_formula_sum            'C32 H36 Cl Fe Ge N2 O4 P'
_chemical_formula_weight         707.49
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-24T22:05:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-05-25 deposited with the CCDC.
2015-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                68.117(10)
_cell_angle_beta                 83.597(14)
_cell_angle_gamma                71.997(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6544(15)
_cell_length_b                   12.518(2)
_cell_length_c                   16.755(3)
_cell_measurement_reflns_used    3442
_cell_measurement_temperature    100
_cell_measurement_theta_max      20.817
_cell_measurement_theta_min      2.571
_cell_volume                     1787.0(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.089
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18364
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.83
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.401
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        SADABS-2008/1 (Bruker,2008) was used for absorption correction.
        wR2(int) was 0.1145 before and 0.0812 after correction.
        The Ratio of minimum to maximum transmission is 0.8491.
        The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.93
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.93
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                3712
_reflns_number_total             6463
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02287h2.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 7036716--7036720.cif.'
_cod_original_cell_volume        1786.9(5)
_cod_database_code               7036717
_platon_squeeze_void_probe_radius 1.20