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_7132382
_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         'C57 H57 O5.25 Rb3'
_chemical_formula_sum            'C57 H57 O5.25 Rb3'
_chemical_formula_weight         1082.43
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-08-21
_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                 92.424(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.4358(3)
_cell_length_b                   15.8158(2)
_cell_length_c                   26.6220(3)
_cell_measurement_reflns_used    12488
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      72.6710
_cell_measurement_theta_min      3.2780
_cell_volume                     10700.1(2)
_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      200.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rigaku Synergy-i'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35064
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         73.205
_diffrn_reflns_theta_min         3.291
_diffrn_source                   'microsource tube'
_exptl_absorpt_coefficient_mu    3.825
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.344
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4416
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         10480
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0948P)^2^+11.1797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6670
_reflns_number_total             10480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05527b2.cif
_cod_data_source_block           wit_exp_820_auto
_cod_depositor_comments
'Adding full bibliography for 7132379--7132383.cif.'
_cod_original_sg_symbol_H-M      C12/c1
_cod_database_code               7132382
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.797
_shelx_estimated_absorpt_t_min   0.651
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{O6, C59}
{O7, C61}
3. Restrained distances
 O4-C52 = O4-C49
 1.43 with sigma of 0.01
 C49-C50 = C50-C51 = C51-C52
 1.53 with sigma of 0.01
 O4-C52A = O4-C49A
 1.43 with sigma of 0.01
 C49A-C50A = C50A-C51A = C51A-C52A
 1.53 with sigma of 0.01
 O6-C60 = O6-C57 = O7-C60 = O7-C58
 1.47 with sigma of 0.01
 C58-C57
 1.53 with sigma of 0.01
 C49A-C51A = C49A-C52A = C49-C52 = C50-C52
 2.4 with sigma of 0.02
 C57-C60 = C58-O6 = C57-O7
 2.4 with sigma of 0.02
 C36-H36A = C36-H36B = C20-H20A = C20-H20B = C4-H4A = C4-H4B
 0.95 with sigma of 0.01
4. Rigid bond restraints
 O4, C49, C50, C51, C52
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O6, C59, C57, C58, C60
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O4 \\sim C49 \\sim C50 \\sim C51 \\sim C52: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.02
O6 \\sim C59 \\sim C57 \\sim C58 \\sim C60: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.02
Uanis(C49) = Uanis(C49A)
Uanis(C50) = Uanis(C50A)
Uanis(C51) = Uanis(C51A)
Uanis(C52) = Uanis(C52A)
Uanis(O6) = Uanis(C59)
Uanis(O7) = Uanis(C61)
6. Others
 Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(C50A)=Sof(H50C)=Sof(H50D)=Sof(C49A)=
 Sof(H49C)=Sof(H49D)=Sof(C52A)=Sof(H52C)=Sof(H52D)=1-FVAR(1)
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(H51A)=
 Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=FVAR(1)
 Fixed Sof: O6(0.125) O7(0.125) C59(0.125) H6A(0.125) H6B(0.125) C57(0.25)
 H57A(0.25) H57B(0.25) C58(0.25) H58A(0.25) H58B(0.25) C60(0.25) H60A(0.25)
 H60B(0.25) C61(0.125) H7A(0.125) H7B(0.125)
7.a Fixed occupancy and ADP/Uiso:
 H4A, H4B, H20A, H20B, H36A, H36B
7.b Riding coordinates:
 C59(H6A,H6B), C57(H57A,H57B), C58(H58A,H58B), C60(H60A,H60B), C61(H7A,H7B)
7.c Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,
 H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C51A(H51C,H51D),
 C50A(H50C,H50D), C49A(H49C,H49D), C52A(H52C,H52D)
7.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34),
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46),
  C47(H47), C48(H48)
;
_shelx_res_checksum              42893
_shelx_hkl_checksum              62044
_olex2_submission_special_instructions 'No special instructions were received'