Hydrogen Bonding to a Dinitrogen Complex at Room Temperature: Impacts on N<sub>2</sub> Activation.
Shanahan, James P.; Szymczak, Nathaniel K.; Journal of the American Chemical Society 141 (2019) 8550–8556; doi:10.1021/jacs.9b02288

data_4128768
_publ_section_title
;
 Hydrogen Bonding to a Dinitrogen Complex at Room Temperature: Impacts on
 N<sub>2</sub> Activation.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8550
_journal_page_last               8556
_journal_paper_doi               10.1021/jacs.9b02288
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C20 H48 Br N2 P4 Re, F6 P'
_chemical_formula_sum            'C20 H48 Br F6 N2 P5 Re'
_chemical_formula_weight         851.56
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-02-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
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_cell_length_c                   14.0353(2)
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_cell_measurement_theta_max      68.7030
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_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      85(2)
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_diffrn_measured_fraction_theta_max 0.983
_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   -110.00  70.00   1.00    1.00    --  -20.00   0.00-180.00  180
  2  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  3  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  4  \w    -25.00  43.00   1.00    1.00    --  -20.00  36.00 120.00   68
  5  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00-180.00   45
  6  \w   -173.00-128.00   1.00    3.00    --  -92.00 -36.00 120.00   45
  7  \w   -133.00 -88.00   1.00    3.00    --  -92.00 -36.00 -60.00   45
  8  \w   -104.00 -59.00   1.00    3.00    --  -92.00  36.00  60.00   45
  9  \w   -122.00 -77.00   1.00    3.00    --  -92.00 -72.00  60.00   45
 10  \w   -174.00 -78.00   1.00    3.00    --  -92.00 -72.00-120.00   96
 11  \w    -93.00 -35.00   1.00    3.00    --  -92.00  36.00-120.00   58
 12  \w   -176.00 -77.00   1.00    3.00    --  -92.00 -72.00 -60.00   99
 13  \w   -147.00 -75.00   1.00    3.00    --  -92.00 -72.00-180.00   72
 14  \w   -176.00 -77.00   1.00    3.00    --  -92.00 -72.00 120.00   99
 15  \w   -177.00-116.00   1.00    3.00    --  -92.00 -36.00  60.00   61
 16  \w    -87.00  -9.00   1.00    3.00    --  -92.00  36.00 -60.00   78
 17  \w   -102.00 -14.00   1.00    3.00    --  -92.00  36.00   0.00   88
 18  \w   -102.00 -21.00   1.00    3.00    --  -92.00  72.00 120.00   81
 19  \w   -175.00-104.00   1.00    3.00    --  -92.00 -36.00   0.00   71
 20  \w   -104.00 -52.00   1.00    3.00    --  -92.00  72.00  60.00   52
 21  \w   -109.00 -14.00   1.00    3.00    --  -92.00  72.00-120.00   95
 22  \w   -105.00 -24.00   1.00    3.00    --  -92.00  36.00-120.00   81
 23  \w   -105.00  -2.00   1.00    3.00    --  -92.00  36.00-180.00  103
 24  \w   -106.00  -2.00   1.00    3.00    --  -92.00  72.00 -60.00  104
 25  \w   -106.00  -2.00   1.00    3.00    --  -92.00  72.00 -60.00  104
 26  \w   -107.00 -29.00   1.00    3.00    --  -92.00  72.00   0.00   78
 27  \w   -117.00 -72.00   1.00    3.00    --  -92.00  72.00 180.00   45
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1215130000
_diffrn_orient_matrix_UB_12      0.0863604000
_diffrn_orient_matrix_UB_13      -0.0435930000
_diffrn_orient_matrix_UB_21      -0.1049305000
_diffrn_orient_matrix_UB_22      -0.1023701000
_diffrn_orient_matrix_UB_23      -0.0151523000
_diffrn_orient_matrix_UB_31      -0.0095139000
_diffrn_orient_matrix_UB_32      0.0211061000
_diffrn_orient_matrix_UB_33      0.1059950000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22434
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.407
_diffrn_reflns_theta_min         4.759
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.240
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_description       block
_exptl_crystal_F_000             842
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.340
_refine_diff_density_min         -1.732
_refine_diff_density_rms         0.231
_refine_ls_extinction_coef       0.0031(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+6.4104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2805
_reflns_number_total             2815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02288_si_002.cif
_cod_data_source_block           jps4060
_cod_database_code               4128768
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C20H48BrF6N2P5Re
_reflns_odcompleteness_completeness 98.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.28
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Br1) = Uanis(N1) = Uanis(N2)
3. Others
 Fixed Sof: Br1(0.5) N1(0.5) N2(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C4(H4A,H4B), C5(H5A,H5B), C8(H8A,H8B), C6(H6A,H6B), C2(H2A,H2B)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              52825
_shelx_hkl_checksum              57839
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 7.707
_oxdiff_exptl_absorpt_empirical_full_min 0.398