Calcium-Based Catalytic System for the Synthesis of Bio-Derived Cyclic Carbonates under Mild Conditions
Longwitz, Lars; Steinbauer, Johannes; Spannenberg, Anke; Werner, Thomas; ACS Catalysis 8 (2017) 665–; doi:10.1021/acscatal.7b03367

data_4514320
_publ_section_title
;
 Calcium-Based Catalytic System for the Synthesis of Bio-Derived Cyclic
 Carbonates under Mild Conditions
;
_journal_issue                   1
_journal_name_full               'ACS Catalysis'
_journal_page_first              665
_journal_paper_doi               10.1021/acscatal.7b03367
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C18 H43.6 Ca I2 N6 O6.8'
_chemical_formula_weight         746.87
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.8605(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5906(2)
_cell_length_b                   22.4298(4)
_cell_length_c                   11.6710(2)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.57
_cell_measurement_theta_min      2.35
_cell_volume                     3225.58(10)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            36482
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.816
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.148
_exptl_absorpt_correction_T_max  0.54
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.496
_exptl_crystal_size_mid          0.431
_exptl_crystal_size_min          0.326
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7787
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+2.2342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6961
_reflns_number_total             7787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b03367_si_003.cif
_cod_data_source_block           AX1230
_cod_depositor_comments
'Adding full bibliography for 4514320--4514321.cif.'
_cod_original_formula_sum        'C18 H43.60 Ca I2 N6 O6.80'
_cod_database_code               4514320
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              50365
_shelx_hkl_checksum              3606