Donor-Acceptor-Stabilized Germanium Analogues of Acid Chloride, Ester, and Acyl Pyrrole Compounds: Synthesis and Reactivity
Sharma, Mahendra Kumar; Sinhababu, Soumen; Mahawar, Pritam; Mukherjee, Goutam; Pandey, Bhawana; Rajaraman, Gopalan; Selvarajan, Nagendran; Chemical Science  (2019) –; doi:10.1039/C8SC05380D

data_1550605
_publ_section_title
;
 Donor-Acceptor-Stabilized Germanium Analogues of Acid Chloride, Ester,
 and Acyl Pyrrole Compounds: Synthesis and Reactivity
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC05380D
_journal_year                    2019
_chemical_formula_moiety         'C41 H28 B F15 Ge N2 O, 0.5(C2 H4 Cl2)'
_chemical_formula_sum            'C42 H30 B Cl F15 Ge N2 O'
_chemical_formula_weight         982.55
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-06-22 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                65.642(3)
_cell_angle_beta                 74.276(3)
_cell_angle_gamma                74.609(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7566(13)
_cell_length_b                   13.7449(15)
_cell_length_c                   13.7689(15)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      26.68
_cell_measurement_theta_min      2.24
_cell_volume                     1920.9(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      104.33
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1800
_diffrn_reflns_av_unetI/netI     0.0930
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34134
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.679
_diffrn_reflns_theta_min         1.828
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       block
_exptl_crystal_F_000             986.0
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   0.822
_exptl_transmission_factor_min   0.763
_refine_diff_density_max         0.889
_refine_diff_density_min         -1.407
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0328P)^2^+3.1313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6794
_reflns_number_total             8074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05380d2.cif
_cod_data_source_block           Compound_17__msh73_0m_a
_cod_database_code               1550605
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C8(H8A,H8B), C42(H42A,H42B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C3(H3), C2(H2), C4(H4), C19(H19), C20(H20), C23(H23),
 C21(H21), C22(H22)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C15(H15A,H15B,
 H15C)
;
_shelx_res_checksum              20265
_olex2_submission_special_instructions 'No special instructions were received'