In situ nano Au triggered by a metal boron organic polymer: efficient electrochemical N2 fixation to NH3 under ambient conditions
Zhao, Xue; Yao, Chen; Chen, Hao; Fu, Yunfan; Xiang, Changjun; He, Suhang; Zhou, Xiaohai; Zhang, Haibo; Journal of Materials Chemistry A 7 (2019) 20945–; doi:10.1039/C9TA06573C

data_7237682
_publ_section_title
;
 In situ nano Au triggered by a metal boron organic polymer: efficient
 electrochemical N2 fixation to NH3 under ambient conditions
;
_journal_issue                   36
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              20945
_journal_paper_doi               10.1039/C9TA06573C
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety
'2(C36 H24 N6 Ni), 3(C3 H7 N O), H2 O, 2(B12 H12)'
_chemical_formula_sum            'C81 H95 B24 N15 Ni2 O4'
_chemical_formula_weight         1719.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-26 deposited with the CCDC.	2019-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                61.953(3)
_cell_angle_beta                 87.914(2)
_cell_angle_gamma                84.292(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8650(4)
_cell_length_b                   18.8050(5)
_cell_length_c                   19.2331(5)
_cell_measurement_reflns_used    13042
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.1660
_cell_measurement_theta_min      3.9930
_cell_volume                     4403.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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   -113.00 -14.00   1.00    1.50    --  -41.14 -57.00  60.00   99
  2  \w    -68.00  30.00   1.00    1.50    --  -41.14  57.00-150.00   98
  3  \w    -91.00  -2.00   1.00    1.50    --  -41.14 125.00 -90.00   89
  4  \w     99.00 174.00   1.00    3.00    --  106.22  30.00 -90.00   75
  5  \w     34.00 117.00   1.00    3.00    --  106.22-125.00 150.00   83
  6  \w    149.00 177.00   1.00    3.00    --  106.22  61.00  60.00   28
  7  \w     81.00 133.00   1.00    3.00    --  106.22  61.00  60.00   52
  8  \w     50.00 116.00   1.00    3.00    --  106.22-125.00 -60.00   66
  9  \w     94.00 177.00   1.00    3.00    --  106.22 125.00 -60.00   83
 10  \w     77.00 169.00   1.00    3.00    --  106.22  77.00 120.00   92
 11  \w     83.00 178.00   1.00    3.00    --  106.22  77.00   0.00   95
 12  \w     30.00 135.00   1.00    3.00    --  106.22 -77.00 -60.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0391813000
_diffrn_orient_matrix_UB_12      0.0802037000
_diffrn_orient_matrix_UB_13      -0.0594524000
_diffrn_orient_matrix_UB_21      -0.0856058000
_diffrn_orient_matrix_UB_22      0.0475269000
_diffrn_orient_matrix_UB_23      0.0178506000
_diffrn_orient_matrix_UB_31      0.0600604000
_diffrn_orient_matrix_UB_32      -0.0007633000
_diffrn_orient_matrix_UB_33      0.0662184000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24908
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        65.998
_diffrn_reflns_theta_max         65.998
_diffrn_reflns_theta_min         3.978
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       block
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1192
_refine_ls_number_reflns         15228
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0934P)^2^+1.4437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12854
_reflns_number_total             15228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ta06573c2.cif
_cod_data_source_block           2
_cod_database_code               7237682
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.843
_reflns_odcompleteness_completeness 99.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 O4, N16, C82, C83, C84, O3, N15, C79, C80, C81
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O4 \\sim N16 \\sim C82 \\sim C83 \\sim C84 \\sim O3 \\sim N15 \\sim C79 \\sim
C80 \\sim C81: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(O3)=Sof(N15)=Sof(C79)=Sof(H79)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=
 Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=1-FVAR(1)
 Sof(O4)=Sof(N16)=Sof(C82)=Sof(H82)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=
 Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=FVAR(1)
5.a Free rotating group:
 O1W(H1WA,H1WB)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46),
  C49(H49), C50(H50), C51(H51), C53(H53), C54(H54), C56(H56), C57(H57),
 C58(H58), C61(H61), C62(H62), C63(H63), C65(H65), C66(H66), C68(H68), C69(H69),
  C70(H70), C73(H73), C76(H76), C82(H82), C79(H79)
5.c Idealised Me refined as rotating group:
 C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C77(H77A,H77B,H77C), C78(H78A,H78B,
 H78C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C80(H80A,H80B,H80C), C81(H81A,
 H81B,H81C)
5.d Boron cage BH refined with riding coordinates:
 B1(H1A), B2(H2A), B3(H3A), B4(H4), B5(H5A), B6(H6A), B7(H7), B8(H8A), B9(H9A),
  B10(H10A), B11(H11), B12(H12), B13(H13A), B14(H14A), B15(H15A), B16(H16),
 B17(H17A), B18(H18A), B19(H19), B20(H20A), B21(H21A), B22(H22A), B23(H23),
 B24(H24)
;
_shelx_res_checksum              16599
_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 2.590
_oxdiff_exptl_absorpt_empirical_full_min 0.508