Pyrrolizidines for Direct Air Capture and CO2 Conversion
Hanusch, Jan M.; Kerschgens, Isabel; Huber, Florian; Neuburger, Markus; Gademann, Karl; Chemical Communications  (2018) –; doi:10.1039/C8CC08574A

data_7122758
_publ_section_title
;
 Pyrrolizidines for Direct Air Capture and CO2 Conversion
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC08574A
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C9 H16 N2 O2), 3(H2 O)'
_chemical_formula_sum            'C18 H38 N4 O7'
_chemical_formula_weight         422.52
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2017-11-07 deposited with the CCDC.
2018-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.952(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8954(8)
_cell_length_b                   22.637(2)
_cell_length_c                   11.6950(11)
_cell_measurement_reflns_used    2197
_cell_measurement_temperature    123
_cell_measurement_theta_max      67
_cell_measurement_theta_min      4
_cell_volume                     2089.9(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15770
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         68.901
_diffrn_reflns_theta_min         3.905
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             919.991
_exptl_crystal_recrystallization_method
; 
 
;
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.25
_refine_ls_abs_structure_details 'Flack (1983), 3072 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.7(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         5647
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.0004738
_refine_ls_shift/su_mean         0.0000335
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.284 0.255 0.127 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0773
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0519
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              -12
_reflns_number_gt                4743
_reflns_number_total             6655
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0542
_oxford_refine_ls_scale          0.1204(2)
_oxford_reflns_number_all        6623
_oxford_reflns_threshold_expression_ref I>1.0\s(I)
_cod_data_source_file            c8cc08574a2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        2089.9(2)
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               7122758