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_1550308
_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 unk
_chemical_formula_moiety         'B0.5 H1.5 O1.5, C39 H45 N2, C H O3'
_chemical_formula_sum            'C40 H47.5 B0.5 N2 O4.5'
_chemical_formula_weight         633.75
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           ' P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3779(19)
_cell_length_b                   14.5134(16)
_cell_length_c                   13.085(2)
_cell_measurement_reflns_used    2018
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      24.8210
_cell_measurement_theta_min      2.0940
_cell_volume                     3680.0(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9160
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -19.00  25.00   1.00  101.43    --  -26.98 -99.00 120.00   44
  2  \w     -1.00 100.00   1.00  101.43    --   28.55  77.00  60.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0214260000
_diffrn_orient_matrix_UB_12      -0.0130201000
_diffrn_orient_matrix_UB_13      -0.0416193000
_diffrn_orient_matrix_UB_21      -0.0170730000
_diffrn_orient_matrix_UB_22      -0.0431021000
_diffrn_orient_matrix_UB_23      -0.0030496000
_diffrn_orient_matrix_UB_31      -0.0243572000
_diffrn_orient_matrix_UB_32      0.0188809000
_diffrn_orient_matrix_UB_33      -0.0345600000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            6541
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.75
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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    1.1438
_exptl_crystal_description       block
_exptl_crystal_F_000             1360.6245
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.2940
_refine_diff_density_min         -0.4850
_refine_diff_density_rms         0.0760
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.5(5)
_refine_ls_d_res_high            0.8404
_refine_ls_d_res_low             11.6165
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0616
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    80
_refine_ls_number_parameters     437
_refine_ls_number_reflns         5474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0616
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          0.0156
_refine_ls_shift/su_mean         0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+6.8814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2081
_refine_ls_wR_factor_ref         0.2179
_reflns_Friedel_coverage         0.652
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              15
_reflns_limit_l_min              -15
_reflns_number_gt                4783
_reflns_number_total             5474
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8sc03581d3.cif
_cod_data_source_block           9BBN_Carbene
_cod_database_code               1550308
_chemical_oxdiff_formula         'C H N O B'
_reflns_odcompleteness_completeness 85.62
_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) groups
2. Others
 Fixed Sof: H5a(0.5)
3.a Ternary CH refined with riding coordinates:
 C18(H18), C36(H36), C21(H21), C39(H39)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C11(H11), C16(H16), C25(H25), C32(H32), C7(H7), C29(H29), C15(H15),
 C27(H27), C33(H33), C28(H28), C9(H9), C14(H14), C26(H26), C34(H34), C8(H8),
 C10(H10)
3.c Idealised Me refined as rotating group:
 C41(H41a,H41b,H41c), C38(H38a,H38b,H38c), C23(H23a,H23b,H23c), C40(H40a,H40b,
 H40c), C20(H20a,H20b,H20c), C37(H37a,H37b,H37c), C19(H19a,H19b,H19c), C22(H22a,
 H22b,H22c)
3.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O5(H5a), O1(H1)
;
_olex2_date_sample_data_collection 2017-06-17
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.197
_oxdiff_exptl_absorpt_empirical_full_min 0.837