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_1560143
_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_formula_sum            'C108 H172 N4 Na4 O12'
_chemical_formula_weight         1810.45
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      cubic
_space_group_IT_number           220
_space_group_name_Hall           'I -4bd 2c 3'
_space_group_name_H-M_alt        'I -4 3 d'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   32.0084(5)
_cell_length_b                   32.0084(5)
_cell_length_c                   32.0084(5)
_cell_measurement_reflns_used    7905
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      68.1933
_cell_measurement_theta_min      3.3822
_cell_volume                     32793.8(9)
_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_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0862
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            42456
_diffrn_reflns_theta_full        68.28
_diffrn_reflns_theta_max         68.28
_diffrn_reflns_theta_min         3.38
_diffrn_source                   'Incoatec Microfocus I\mS'
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11856
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.133
_refine_diff_density_min         -0.176
_refine_ls_abs_structure_details
;

Flack x determined using 1984 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         5015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0739
_reflns_number_gt                4523
_reflns_number_total             5015
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06851a2.cif
_cod_data_source_block           3
_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_cell_volume        32793.8(15)
_cod_database_code               1560143
_shelx_res_checksum              54919
_shelx_hkl_checksum              41148
_shelx_fab_checksum              48533