Bis(chlorogermyliumylidene) and its significant role in elusive reductive cyclization.
Majumdar, Moumita; Raut, Ravindra K.; Sahoo, Padmini; Kumar, Vikas; Chemical communications (Cambridge, England) 54 (2018) 10839–10842; doi:10.1039/c8cc06067c

data_7122277
_publ_section_title
;
 Bis(chlorogermyliumylidene) and its significant role in elusive reductive
 cyclization.
;
_journal_issue                   77
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10839
_journal_page_last               10842
_journal_paper_doi               10.1039/c8cc06067c
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C40 H66 K2 N4 O12'
_chemical_formula_weight         873.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-05-21 deposited with the CCDC.
2018-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.411(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.5972(19)
_cell_length_b                   14.6704(10)
_cell_length_c                   26.824(2)
_cell_measurement_reflns_used    2848
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      59.68
_cell_measurement_theta_min      2.88
_cell_volume                     8993.8(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2375
_diffrn_reflns_av_unetI/netI     0.4093
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            59611
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        66.932
_diffrn_reflns_theta_max         66.932
_diffrn_reflns_theta_min         2.234
_exptl_absorpt_coefficient_mu    2.382
_exptl_absorpt_correction_T_max  0.189
_exptl_absorpt_correction_T_min  0.152
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.75
_exptl_crystal_size_min          0.58
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 1386 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.18(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2097
_refine_ls_number_reflns         30226
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.3799
_refine_ls_R_factor_gt           0.1133
_refine_ls_shift/su_max          1.718
_refine_ls_shift/su_mean         0.145
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+0.4753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1936
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    0.895
_reflns_Friedel_fraction_max     0.895
_reflns_number_gt                6710
_reflns_number_total             30226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc06067c2.cif
_cod_data_source_block           Lr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

 Adding full bibliography for 7122274--7122277.cif.
;
_cod_original_cell_volume        8993.9(12)
_cod_database_code               7122277
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              99953