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_1550306
_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_formula_moiety         'C47 H59 B N2'
_chemical_formula_sum            'C47 H59 B N2'
_chemical_formula_weight         662.77
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_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                 98.7643(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2461(3)
_cell_length_b                   23.0691(6)
_cell_length_c                   15.3687(3)
_cell_measurement_reflns_used    4362
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      27.9320
_cell_measurement_theta_min      2.0190
_cell_volume                     3940.66(17)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9160
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.881
_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    -40.00  67.00   1.00   55.00    --   28.47 -57.00 -90.00  107
  2  \w     -8.00 107.00   1.00   55.00    --   28.47  77.00 120.00  115
;
_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      0.0577459000
_diffrn_orient_matrix_UB_12      -0.0032004000
_diffrn_orient_matrix_UB_13      -0.0125817000
_diffrn_orient_matrix_UB_21      -0.0113403000
_diffrn_orient_matrix_UB_22      -0.0299096000
_diffrn_orient_matrix_UB_23      -0.0079754000
_diffrn_orient_matrix_UB_31      -0.0246755000
_diffrn_orient_matrix_UB_32      0.0062814000
_diffrn_orient_matrix_UB_33      -0.0442946000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13082
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.12
_diffrn_reflns_theta_min         2.03
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89500
_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    1.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         8482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+2.2202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                6694
_reflns_number_total             8482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8sc03581d3.cif
_cod_data_source_block           solidair
_cod_original_cell_volume        3940.67(15)
_cod_database_code               1550306
_chemical_oxdiff_formula         'C H N O B'
_reflns_odcompleteness_completeness 98.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C21(H21), C18(H18), C42(H42), C46(H46), C36(H36), B1(H1), C39(H39)
2.b Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C43(H43A,H43B), C45(H45A,H45B), C48(H48A,H48B), C44(H44A,
 H44B), C47(H47A,H47B)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C29(H29), C11(H11), C10(H10), C26(H26), C32(H32), C16(H16),
 C28(H28), C7(H7), C14(H14), C9(H9), C25(H25), C8(H8), C33(H33), C27(H27),
 C34(H34)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C41(H41A,H41B,H41C), C22(H22A,H22B,
 H22C), C20(H20A,H20B,H20C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,
 H40B,H40C)
;
_olex2_date_sample_data_collection 2016-10-04
_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 1.309
_oxdiff_exptl_absorpt_empirical_full_min 0.690