Efficient synthesis of cyclic carbonates and oxazolidinones by simple zinc guanidinato complexes.
Ginés, Carlos; Parra-Cadenas, Blanca; Elorriaga, David; García-Vivó, Daniel; Fernández-Galán, Rafael; Ramos, Alberto; Carrillo-Hermosilla, Fernando; Dalton transactions (Cambridge, England : 2003) 55 (2026) 4525–4534; doi:10.1039/d6dt00139d

data_7720263
_publ_section_title
;
 Efficient synthesis of cyclic carbonates and oxazolidinones by simple
 zinc guanidinato complexes.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4525
_journal_page_last               4534
_journal_paper_doi               10.1039/d6dt00139d
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C28 H46 N6 O2 Zn2'
_chemical_formula_sum            'C28 H46 N6 O2 Zn2'
_chemical_formula_weight         629.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2qlzmy
_audit_creation_date             2025-11-27
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-01-06 deposited with the CCDC.	2026-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.7640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.50200(10)
_cell_length_b                   10.97330(10)
_cell_length_c                   15.7972(2)
_cell_measurement_reflns_used    19929
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      68.0500
_cell_measurement_theta_min      2.8880
_cell_volume                     1592.76(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.144a (release 23-01-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_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   -120.00 -19.00   0.50    0.05    --  -88.35  79.00 146.00  202
  2  \w    -32.00  -6.00   0.50    0.05    --  -88.35  30.00  60.00   52
  3  \w    -32.00  -6.00   0.50    0.05    --  -88.35  30.00   0.00   52
  4  \w    -47.00  -7.00   0.50    0.05    --  -88.35  45.00 -30.00   80
  5  \w    -47.00  -7.00   0.50    0.05    --  -88.35  45.00 -90.00   80
  6  \w    -23.00  78.00   0.50    0.05    --   46.07 -79.00  22.00  202
  7  \w    -23.00  78.00   0.50    0.05    --   46.07 -79.00  22.00  202
  8  \w    -36.00  30.00   0.50    0.05    --   46.07 -19.00  60.00  132
  9  \w    -36.00  30.00   0.50    0.05    --   46.07 -19.00 120.00  132
 10  \w     36.00 138.00   0.50    0.05    --  105.50 -79.00  22.00  204
 11  \w     44.00 145.00   0.50    0.05    --  113.15 -79.00  22.00  202
 12  \w     36.00  75.00   0.50    0.05    --  113.15 -61.00 150.00   78
 13  \w     35.00 109.00   0.50    0.05    --  105.50 -77.00  90.00  148
 14  \w     25.00  54.00   0.50    0.05    --  105.50 -45.00  30.00   58
 15  \w     25.00  54.00   0.50    0.05    --  105.50 -45.00   0.00   58
 16  \w     25.00  54.00   0.50    0.05    --  105.50 -45.00 -30.00   58
 17  \w     25.00  54.00   0.50    0.05    --  105.50 -45.00 -60.00   58
 18  \w     35.00 109.00   0.50    0.05    --  105.50 -77.00 -90.00  148
 19  \w     40.00 105.00   0.50    0.05    --  113.15 -95.00-120.00  130
 20  \w     42.00 103.00   0.50    0.05    --  113.15 -95.00   0.00  122
 21  \w    -23.00  35.00   0.50    0.05    --  -47.32  19.00 150.00  116
 22  \w    -79.00  22.00   0.50    0.05    --  -47.32  79.00 146.00  202
 23  \w    -23.00  35.00   0.50    0.05    --  -47.32  19.00-150.00  116
 24  \w     75.00 178.00   0.50    0.05    --  105.50  30.00-120.00  206
 25  \w     93.00 177.00   0.50    0.05    --  113.15  61.00-150.00  168
 26  \w     81.00 178.00   0.50    0.05    --  105.50  61.00  90.00  194
 27  \w    134.00 177.00   0.50    0.05    --  113.15  79.00 146.00   86
 28  \w     86.00 178.00   0.50    0.05    --  113.15  79.00 146.00  184
 29  \w     86.00 175.00   0.50    0.05    --  105.50  79.00 146.00  178
 30  \w    151.00 176.00   0.50    0.05    --  113.15  45.00 120.00   50
 31  \w     93.00 178.00   0.50    0.05    --  113.15  45.00  90.00  170
 32  \w     95.00 120.00   0.50    0.05    --  113.15  45.00 120.00   50
 33  \w     86.00 178.00   0.50    0.05    --  105.50  45.00 -90.00  184
 34  \w     86.00 178.00   0.50    0.05    --  105.50  45.00 -90.00  184
 35  \w     75.00 178.00   0.50    0.05    --  105.50  30.00-120.00  206
 36  \w   -171.00 -58.00   0.50    0.05    --  -88.35 -30.00 -90.00  226
 37  \w   -171.00 -58.00   0.50    0.05    --  -88.35 -30.00 -90.00  226
 38  \w   -112.00 -13.00   0.50    0.05    --  -88.35 125.00  60.00  198
 39  \w   -158.00 -79.00   0.50    0.05    --  -88.35 -79.00  22.00  158
 40  \w   -158.00 -79.00   0.50    0.05    --  -88.35 -79.00  22.00  158
 41  \w   -162.00 -84.00   0.50    0.05    --  -88.35 -95.00 -60.00  156
 42  \w   -123.00 -74.00   0.50    0.05    --  -47.32-125.00 150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1340652000
_diffrn_orient_matrix_UB_12      -0.0107260000
_diffrn_orient_matrix_UB_13      0.0375484000
_diffrn_orient_matrix_UB_21      0.0611187000
_diffrn_orient_matrix_UB_22      -0.1192953000
_diffrn_orient_matrix_UB_23      0.0464310000
_diffrn_orient_matrix_UB_31      0.0800089000
_diffrn_orient_matrix_UB_32      0.0731868000
_diffrn_orient_matrix_UB_33      0.0812944000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0094
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28765
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.346
_diffrn_reflns_theta_min         4.944
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.106
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.144a (Rigaku Oxford Diffraction, 2024)
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    1.312
_exptl_crystal_description       plate
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0228
_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^)+(0.0345P)^2^+0.4219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2790
_reflns_number_total             2921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00139d2.cif
_cod_data_source_block           04329
_cod_depositor_comments
'Adding full bibliography for 7720261--7720263.cif.'
_cod_database_code               7720263
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C14H23N3Zn
_chemical_oxdiff_usercomment     'CG149 250K'
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.754
_diffrn_oxdiff_digest_hkl
;
4349dacc60e0d965ef255e9b10add172df5893
;
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C2(H2), C11(H11)
1.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10)
1.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              6821
_shelx_hkl_checksum              40371
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.262
_oxdiff_exptl_absorpt_empirical_full_min 0.886