Isolable rubidium and caesium derivatives of common organic carbonyl compounds.
Wacker, Jakoba; Lynch, Jennifer R.; Banerjee, Sumanta; Macdonald, Peter A.; Kennedy, Alan R.; Sarkar, Biprajit; Mulvey, Robert E.; Chemical communications (Cambridge, England) 60 (2023) 91–94; doi:10.1039/d3cc05527b

data_7132381
_publ_section_title
;
 Isolable rubidium and caesium derivatives of common organic carbonyl
 compounds.
;
_journal_issue                   1
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              91
_journal_page_last               94
_journal_paper_doi               10.1039/d3cc05527b
_journal_volume                  60
_journal_year                    2023
_chemical_formula_moiety         '0.25(C56 H48 Cs4 N4 O4)'
_chemical_formula_sum            'C14 H12 Cs N O'
_chemical_formula_weight         343.16
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-09-05 deposited with the CCDC.	2023-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.6607(4)
_cell_length_b                   6.0929(2)
_cell_length_c                   22.6838(7)
_cell_measurement_reflns_used    24994
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      72.9910
_cell_measurement_theta_min      3.8840
_cell_volume                     2579.10(13)
_computing_cell_refinement       CrysalisPro
_computing_data_collection       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Rigaky Synegy-i'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37960
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         74.464
_diffrn_reflns_theta_min         3.897
_diffrn_source                   'microsource tube'
_exptl_absorpt_coefficient_mu    22.254
_exptl_absorpt_correction_T_max  0.474
_exptl_absorpt_correction_T_min  0.216
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_description       plate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.478(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5087
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+7.6930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1147
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                4496
_reflns_number_total             5087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05527b2.cif
_cod_data_source_block           jw-78_1_auto
_cod_depositor_comments
'Adding full bibliography for 7132379--7132383.cif.'
_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               7132381
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.305
_shelx_estimated_absorpt_t_min   0.214
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.522(15)
 0.478(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C18(H18A,H18B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30)
;
_shelx_res_checksum              85545
_shelx_hkl_checksum              30649
_olex2_submission_special_instructions 'No special instructions were received'