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_7132380
_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         'C14 H12 N O Rb'
_chemical_formula_sum            'C14 H12 N O Rb'
_chemical_formula_weight         295.72
_chemical_properties_physical
;
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-05-10
_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                 113.878(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6999(1)
_cell_length_b                   8.7124(1)
_cell_length_c                   12.2028(1)
_cell_measurement_reflns_used    20760
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      72.8880
_cell_measurement_theta_min      3.7910
_cell_volume                     1234.63(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -105.00 -20.00   0.50    0.40    --  -38.83 -49.00-102.00  170
  2  \w    -55.00  28.00   0.50    0.40    --  -38.83  49.00  44.00  166
  3  \w     85.00 171.00   0.50    1.80    --  104.00  49.00  44.00  172
  4  \w    -66.00  30.00   0.50    0.40    --  -38.83  77.00-150.00  192
  5  \w    -78.00  -2.00   0.50    0.40    --  -38.83 112.00   0.00  152
  6  \w   -113.00 -41.00   0.50    0.40    --  -38.83-178.00 120.00  144
  7  \w    -43.00  27.00   0.50    0.40    --  -38.83  38.00-150.00  140
  8  \w   -105.00 -23.00   0.50    0.40    --  -38.83 -38.00-150.00  164
  9  \w    -62.00  29.00   0.50    0.40    --  -38.83  64.00 120.00  182
 10  \w    -31.00  31.00   0.50    0.40    --  -38.83  25.00  90.00  124
 11  \w   -114.00  -4.00   0.50    0.40    --  -38.83 -12.00 -90.00  220
 12  \w   -118.00 -38.00   0.50    0.40    --  -38.83 178.00  30.00  160
 13  \w   -114.00  -4.00   0.50    0.40    --  -38.83 -12.00 -90.00  220
 14  \w    -31.00  31.00   0.50    0.40    --   38.83 -25.00 120.00  124
 15  \w     11.00  43.00   0.50    0.40    --   38.83  80.00-100.44   64
 16  \w    -27.00  55.00   0.50    0.40    --   38.83 -49.00-102.00  164
 17  \w     11.00  43.00   0.50    0.40    --   38.83  80.00 121.91   64
 18  \w     20.00 105.00   0.50    0.40    --   38.83  49.00  44.00  170
 19  \w    -36.00  24.00   0.50    0.40    --   38.83 -12.00-120.00  120
 20  \w    -68.00 -36.00   0.50    1.80    -- -104.00  59.00-150.00   64
 21  \w   -110.00 -40.00   0.50    1.80    -- -104.00 117.00   0.00  140
 22  \w   -106.00 -30.00   0.50    1.80    -- -104.00  96.00 -90.00  152
 23  \w   -170.00 -59.00   0.50    1.80    -- -104.00-145.00 -60.00  222
 24  \w   -174.00 -90.00   0.50    1.80    -- -104.00 -25.00 150.00  168
 25  \w   -127.00 -35.00   0.50    1.80    -- -104.00 145.00 150.00  184
 26  \w   -110.00 -40.00   0.50    1.80    -- -104.00 117.00  90.00  140
 27  \w   -171.00 -85.00   0.50    1.80    -- -104.00 -50.00  90.00  172
 28  \w    -68.00 -36.00   0.50    1.80    -- -104.00  59.00-120.00   64
 29  \w    -68.00 -36.00   0.50    1.80    -- -104.00  59.00-180.00   64
 30  \w   -172.00 -82.00   0.50    1.80    -- -104.00 -59.00 -60.00  180
 31  \w    -83.00 -36.00   0.50    1.80    -- -104.00  68.00 -90.00   94
 32  \w   -171.00 -85.00   0.50    1.80    -- -104.00 -50.00-150.00  172
 33  \w   -172.00 -77.00   0.50    1.80    -- -104.00 -76.00 125.96  190
 34  \w   -127.00 -35.00   0.50    1.80    -- -104.00 145.00  90.00  184
 35  \w   -174.00 -90.00   0.50    1.80    -- -104.00 -25.00  30.00  168
 36  \w    -83.00 -36.00   0.50    1.80    -- -104.00  68.00  90.00   94
 37  \w   -172.00 -80.00   0.50    1.80    -- -104.00 -68.00  30.00  184
 38  \w   -106.00 -30.00   0.50    1.80    -- -104.00  96.00-120.00  152
 39  \w   -114.00 -38.00   0.50    1.80    -- -104.00 127.00  46.71  152
 40  \w   -172.00 -63.00   0.50    1.80    -- -104.00-139.00 161.41  218
 41  \w   -127.00 -35.00   0.50    1.80    -- -104.00 145.00 -90.00  184
 42  \w   -171.00 -81.00   0.50    1.80    -- -104.00-110.00-109.65  180
 43  \w   -174.00 -90.00   0.50    1.80    -- -104.00 -25.00 120.00  168
 44  \w   -105.00 -35.00   0.50    1.80    -- -104.00  77.00  30.00  140
 45  \w   -109.00 -39.00   0.50    1.80    -- -104.00 113.00 -82.81  140
 46  \w   -171.00 -85.00   0.50    1.80    -- -104.00 -50.00  60.00  172
 47  \w   -168.00 -78.00   0.50    1.80    -- -104.00-117.00-180.00  180
 48  \w   -170.00 -85.00   0.50    1.80    -- -104.00 -49.00-102.00  170
 49  \w   -168.00 -76.00   0.50    1.80    -- -104.00-120.00-104.06  184
 50  \w   -172.00 -80.00   0.50    1.80    -- -104.00 -68.00   0.00  184
 51  \w   -172.00 -90.00   0.50    1.80    -- -104.00 -33.00 120.00  164
 52  \w     36.00  68.00   0.50    1.80    --  104.00 -59.00  90.00   64
 53  \w     34.00 135.00   0.50    1.80    --  104.00 -87.00  90.00  202
 54  \w     31.00 106.00   0.50    1.80    --  104.00 -96.00 -60.00  150
 55  \w     36.00  83.00   0.50    1.80    --  104.00 -68.00 -30.00   94
 56  \w     85.00 171.00   0.50    1.80    --  104.00  50.00-150.00  172
 57  \w     31.00 106.00   0.50    1.80    --  104.00 -96.00 -90.00  150
 58  \w     36.00  68.00   0.50    1.80    --  104.00 -59.00-150.00   64
 59  \w     40.00 110.00   0.50    1.80    --  104.00-117.00  90.00  140
 60  \w    -43.00  -7.00   0.50    0.40    --  -38.83 -90.00 100.67   72
 61  \w   -107.00 -12.00   0.50    0.40    --  -38.83 -77.00 120.00  190
 62  \w    -43.00 -10.00   0.50    0.40    --  -38.83 -82.00 -79.07   66
 63  \w    -43.00  -9.00   0.50    0.40    --  -38.83 -86.00-133.20   68
 64  \w   -107.00 -12.00   0.50    0.40    --  -38.83 -77.00  60.00  190
 65  \w   -105.00 -23.00   0.50    0.40    --  -38.83 -38.00 -60.00  164
 66  \w    -43.00  -9.00   0.50    0.40    --  -38.83 -86.00 -12.48   68
 67  \w   -106.00 -16.00   0.50    0.40    --  -38.83 -64.00  90.00  180
 68  \w   -106.00 -16.00   0.50    0.40    --  -38.83 -64.00 150.00  180
 69  \w    -43.00 -11.00   0.50    0.40    --  -38.83 -79.00  18.09   64
 70  \w   -105.00 -23.00   0.50    0.40    --  -38.83 -38.00 150.00  164
 71  \w    -24.00  37.00   0.50    0.40    --  -38.83  12.00  30.00  122
 72  \w    -35.00  -6.00   0.50    0.40    --  -38.83 -94.00-123.73   58
 73  \w     41.00 113.00   0.50    0.40    --   38.83 178.00   0.00  144
 74  \w      9.00  43.00   0.50    0.40    --   38.83  86.00  16.96   68
 75  \w     12.00 108.00   0.50    0.40    --   38.83  77.00 -30.00  192
 76  \w     11.00  43.00   0.50    0.40    --   38.83  81.00-160.07   64
 77  \w     24.00 105.00   0.50    0.40    --   38.83  38.00-150.00  162
 78  \w      9.00  43.00   0.50    0.40    --   38.83  85.00  91.99   68
 79  \w      3.00  79.00   0.50    0.40    --   38.83-112.00  30.00  152
 80  \w      6.00  35.00   0.50    0.40    --   38.83  93.00 -52.45   58
 81  \w   -172.00 -80.00   0.50    1.80    -- -104.00 -68.00 -30.00  184
 82  \w     77.00 149.00   0.50    1.80    --  104.00  77.00 -30.00  144
 83  \w     80.00 172.00   0.50    1.80    --  104.00  68.00-120.00  184
 84  \w     77.00 173.00   0.50    1.80    --  104.00  77.00 150.00  192
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0695159000
_diffrn_orient_matrix_UB_12      0.1330036000
_diffrn_orient_matrix_UB_13      0.0210650000
_diffrn_orient_matrix_UB_21      0.0393885000
_diffrn_orient_matrix_UB_22      -0.0491688000
_diffrn_orient_matrix_UB_23      0.1319222000
_diffrn_orient_matrix_UB_31      0.1058821000
_diffrn_orient_matrix_UB_32      0.1057170000
_diffrn_orient_matrix_UB_33      0.0347544000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0096
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25780
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         73.029
_diffrn_reflns_theta_min         3.806
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.360
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
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    1.591
_exptl_crystal_description       irregular
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0302P)^2^+0.7162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2378
_reflns_number_total             2459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05527b2.cif
_cod_data_source_block           jrl3-101_auto_smart
_cod_depositor_comments
'Adding full bibliography for 7132379--7132383.cif.'
_cod_original_sg_symbol_H-M      P121/c1
_cod_database_code               7132380
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'N H C O Si Rb'
_shelx_estimated_absorpt_t_max   0.616
_shelx_estimated_absorpt_t_min   0.481
_reflns_odcompleteness_completeness 97.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14)
;
_shelx_res_checksum              60926
_shelx_hkl_checksum              81866
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.385
_oxdiff_exptl_absorpt_empirical_full_min 0.790