Soluble, crystalline, and thermally stable alkali CO2− and carbonite (CO22−) clusters supported by cyclic(alkyl)(amino) carbenes
Freeman, Lucas A.; Obi, Akachukwu D.; Machost, Haleigh R.; Molino, Andrew; Nichols, Asa W.; Dickie, Diane A.; Wilson, David J. D.; Machan, Charles W.; Gilliard, Robert J.; Chemical Science 12 (2021) 3544–3550; doi:10.1039/D0SC06851A

data_1560145
_publ_section_title
;
 Soluble, crystalline, and thermally stable alkali CO2&#x2212; and
 carbonite (CO22&#x2212;) clusters supported by cyclic(alkyl)(amino)
 carbenes
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              3544
_journal_page_last               3550
_journal_paper_doi               10.1039/D0SC06851A
_journal_volume                  12
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_sum            'C77 H121 Li6 N3 O8'
_chemical_formula_weight         1258.40
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_update_record
;
2020-03-19 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.449(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2409(17)
_cell_length_b                   14.1749(17)
_cell_length_c                   20.804(2)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      25.4380
_cell_measurement_theta_min      2.4521
_cell_volume                     4066.7(8)
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service v2017.5.0.0'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_unetI/netI     0.1018
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            58000
_diffrn_reflns_theta_full        25.76
_diffrn_reflns_theta_max         25.76
_diffrn_reflns_theta_min         1.01
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1372
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexanes and THF'
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.262
_exptl_crystal_size_min          0.148
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.262
_refine_ls_abs_structure_details
;

Flack x determined using 3082 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(6)
_refine_ls_extinction_coef       0.0096(11)
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     876
_refine_ls_number_reflns         14941
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1305
_refine_ls_R_factor_gt           0.0713
_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^)+(0.0797P)^2^+2.5408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1863
_reflns_number_gt                9446
_reflns_number_total             14941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06851a2.cif
_cod_data_source_block           6
_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/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1560139--1560146.cif.
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1560145
_shelx_res_checksum              88243
_shelx_hkl_checksum              33702
_shelx_fab_checksum              16544