A stable free tetragermacyclobutadiene incorporating fused-ring bulky EMind groups.
Suzuki, Katsunori; Numata, Yasuyuki; Fujita, Naoko; Hayakawa, Naoki; Tanikawa, Tomoharu; Hashizume, Daisuke; Tamao, Kohei; Fueno, Hiroyuki; Tanaka, Kazuyoshi; Matsuo, Tsukasa; Chemical communications (Cambridge, England) 54 (2018) 2200–2203; doi:10.1039/c7cc09443d

data_7121142
_publ_section_title
;
 A stable free tetragermacyclobutadiene incorporating fused-ring bulky
 EMind groups.
;
_journal_issue                   18
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2200
_journal_page_last               2203
_journal_paper_doi               10.1039/c7cc09443d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C96 H148 Ge4, 0.5(C6 H14)'
_chemical_formula_sum            'C99 H155 Ge4'
_chemical_formula_weight         1635.58
_chemical_melting_point          617.0(10)
_chemical_name_common            'Ge CBD'
_chemical_name_systematic        tetragermacyclobutadiene
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-09-20 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                84.4742(5)
_cell_angle_beta                 83.1749(6)
_cell_angle_gamma                87.3583(8)
_cell_formula_units_Z            2
_cell_length_a                   10.3376(1)
_cell_length_b                   17.8421(2)
_cell_length_c                   25.5819(3)
_cell_measurement_reflns_used    264421
_cell_measurement_temperature    90
_cell_measurement_theta_max      33.371
_cell_measurement_theta_min      1.340
_cell_volume                     4660.37(9)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics    SV
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku AFC-8 with Saturn70 CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            264416
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.371
_diffrn_reflns_theta_min         1.340
_diffrn_source                   'Fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    1.320
_exptl_absorpt_correction_T_max  0.93689
_exptl_absorpt_correction_T_min  0.83842
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
 Analytical Absorption Correction Program
 N.W. Alcock (1970). Cryst. Computing, 271
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       plate
_exptl_crystal_F_000             1754
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane and toluene'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         35880
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+0.9394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23868
_reflns_number_total             35880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09443d2.cif
_cod_data_source_block           ge4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '616-618' was changed to '617.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7121142--7121143.cif.
;
_cod_database_code               7121142
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.837
_shelx_estimated_absorpt_t_max   0.937
_shelx_res_checksum              31878