s-Block Carbodicarbene Chemistry: C(sp3)−H Activation and Cyclization Mediated by a Beryllium Center
Walley, Jacob; Breiner, Grace; Wang, Guocang; Dickie, Diane Amanda; Molino, Andrew; Dutton, Jason Laurence; Wilson, David John; Gilliard, Robert J.; Chemical Communications  (2019) –; doi:10.1039/C8CC10022E

data_7122806
_publ_section_title
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 s-Block Carbodicarbene Chemistry: C(sp3)&#x2212;H Activation and
 Cyclization Mediated by a Beryllium Center
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC10022E
_journal_year                    2019
_chemical_formula_sum            'C36 H54 Be Cl N5 Si2'
_chemical_formula_weight         657.48
_chemical_melting_point          340
_chemical_name_common            BeCl(NTMS2)(CDC)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_update_record
;
2018-11-21 deposited with the CCDC.
2019-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.557(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0264(6)
_cell_length_b                   24.8747(19)
_cell_length_c                   16.8657(12)
_cell_measurement_reflns_used    8700
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      27.8091
_cell_measurement_theta_min      2.4153
_cell_volume                     3786.7(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service v2017.5.0.0'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45014
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.46
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.195
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexanes, toluene'
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.281
_exptl_crystal_size_min          0.228
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         9419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0427P)^2^+1.7784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                6910
_reflns_number_total             9419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc10022e2.cif
_cod_data_source_block           2
_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 
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_cod_database_code               7122806
_shelx_res_checksum              28768
_shelx_hkl_checksum              42676