Cleavage of Ge‒Ge and Sn‒Sn Triple Bonds in Heavy Group 14 Element Alkyne Analogues (EAriPr4)2 (E = Ge, Sn; AriPr4 = C6H3-2,6(C6H3-2,6-iPr2)2) by Reaction with Group 6 Carbonyls
McCrea-Hendrick, Madison L.; Caputo, Christine A.; Linnera, Jarno; Vasko, Petra; Weinstein, Cory M.; Fettinger, James C.; Tuononen, Heikki M.; Power, Philip P.; Organometallics 35 (2016) 2759–; doi:10.1021/acs.organomet.6b00519

data_4088869
_publ_section_title
;
 Cleavage of Ge--Ge and Sn--Sn Triple Bonds in Heavy Group 14 Element
 Alkyne Analogues (EAriPr4)2 (E = Ge, Sn; AriPr4 =
 C6H3-2,6(C6H3-2,6-iPr2)2) by Reaction with Group 6 Carbonyls
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              2759
_journal_paper_doi               10.1021/acs.organomet.6b00519
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C68 H74 Cr2 O8 Sn2, 2(C7 H8)'
_chemical_formula_sum            'C82 H90 Cr2 O8 Sn2'
_chemical_formula_weight         1544.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.0130(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5774(5)
_cell_length_b                   25.8862(10)
_cell_length_c                   22.9210(9)
_cell_measurement_reflns_used    5580
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      21.68
_cell_measurement_theta_min      2.34
_cell_volume                     7349.0(5)
_computing_cell_refinement       'SAINT (8.34a) (Bruker, 2013)'
_computing_data_collection       'Apex2 (2010-11.3) (Bruker, 2010)'
_computing_data_reduction        'SAINT (8.34a) (Bruker, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.2004
_diffrn_reflns_av_unetI/netI     0.1594
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            63467
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.276
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_T_max  0.9316
_exptl_absorpt_correction_T_min  0.6649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/3 (Sheldrick, 2014)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       Block
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.00026(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         16884
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.1481
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0280P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9019
_reflns_number_total             16884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00519_si_001.cif
_cod_data_source_block           CC39FMI
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088869
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.951
_shelx_res_checksum              69357
_shelx_hkl_checksum              15603