Transforming Atmospheric CO2 into Alternative Fuels: a Metal-Free Approach under Ambient Conditions
Mandal, Swadhin K.; Sau, Samaresh Ch; Bhattacharjee, Rameswar; Hota, Pradip kumar; Vardhanapu, Pavan Kumar; vijaykumar, gonela; Govindarajan, R.; Datta, Ayan; Chemical Science  (2019) –; doi:10.1039/C8SC03581D

data_1550309
_publ_section_title
;
 Transforming Atmospheric CO2 into Alternative Fuels: a Metal-Free
 Approach under Ambient Conditions
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC03581D
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C39 H45 N2, Cl, H2 O'
_chemical_formula_sum            'C39 H47 Cl N2 O'
_chemical_formula_weight         595.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-09-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-31 deposited with the CCDC.
2018-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.4291(7)
_cell_length_b                   13.1243(4)
_cell_length_c                   14.5076(6)
_cell_measurement_reflns_used    6226
_cell_measurement_temperature    295
_cell_measurement_theta_max      29.1380
_cell_measurement_theta_min      3.5945
_cell_volume                     3508.9(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      295
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_details
;
  1 omega  -23.00    4.00   1.0000   46.0400
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -99.0000  120.0000 27

  2 omega  -94.00  -59.00   1.0000   46.0400
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  178.0000   60.0000 35

  3 omega   -3.00   23.00   1.0000   46.0400
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -97.0000   28.0000 26

  4 omega  -42.00   21.00   1.0000   46.0400
omega____ theta____ kappa____ phi______ frames
    -      -17.3397   37.0000  -30.0000 63

  5 omega  -57.00  -27.00   1.0000   46.0400
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -77.0000  -30.0000 30

  6 omega  -12.00   13.00   1.0000   46.0400
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -77.0000  -30.0000 25

  7 omega  -28.00   -1.00   1.0000   46.0400
omega____ theta____ kappa____ phi______ frames
    -      -17.3397   97.0000  151.0000 27

  8 omega   24.00   53.00   1.0000   46.0400
omega____ theta____ kappa____ phi______ frames
    -      -17.3397   36.0000  129.0000 29

  9 omega   16.00   48.00   1.0000   46.0400
omega____ theta____ kappa____ phi______ frames
    -      -17.3397   57.0000  -30.0000 32

 10 omega  -85.00  -53.00   1.0000   46.0400
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -37.0000  -30.0000 32

 11 omega   27.00   53.00   1.0000   46.0400
omega____ theta____ kappa____ phi______ frames
    -      -17.3397   37.0000  150.0000 26
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0373088000
_diffrn_orient_matrix_UB_12      0.0122535000
_diffrn_orient_matrix_UB_13      -0.0045898000
_diffrn_orient_matrix_UB_21      -0.0006795000
_diffrn_orient_matrix_UB_22      0.0173017000
_diffrn_orient_matrix_UB_23      0.0462971000
_diffrn_orient_matrix_UB_31      0.0094148000
_diffrn_orient_matrix_UB_32      0.0497336000
_diffrn_orient_matrix_UB_33      -0.0149875000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23112
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.20
_diffrn_reflns_theta_min         4.42
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.029
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(6)
_refine_ls_extinction_coef       0.0026(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         7869
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.3635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1208
_reflns_number_gt                5680
_reflns_number_total             7869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8sc03581d3.cif
_cod_data_source_block           bm-dd-4-s
_cod_database_code               1550309
_chemical_oxdiff_formula         'C12 H20 N4 O6'
_chemical_oxdiff_usercomment     'COLOURLESS BLOCK, 295K, 0.75 0.44 0.42'
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B)
2.b Ternary CH refined with riding coordinates:
 C15(H15), C30(H30), C33(H33), C12(H12)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C38(H38), C22(H22), C23(H23), C19(H19), C37(H37), C28(H28), C41(H41),
 C27(H27), C40(H40), C8(H8), C26(H26), C39(H39), C9(H9), C21(H21), C10(H10),
 C20(H20)
2.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C14(H14A,H14B,H14C), C13(H13A,
 H13B,H13C)
;
_olex2_submission_special_instructions 'No special instructions were received'