1,2-Addition and cycloaddition reactions of niobium bis(imido) and oxo imido complexes
Fostvedt, Jade I.; Grant, Lauren N.; Kriegel, Benjamin M.; Obenhuber, Andreas H.; Lohrey, Trevor D.; Bergman, Robert G.; Arnold, John; Chemical Science  (2020) –; doi:10.1039/D0SC03489D

data_1559321
_publ_section_title
;
 1,2-Addition and cycloaddition reactions of niobium bis(imido) and oxo
 imido complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03489D
_journal_year                    2020
_chemical_formula_moiety         'C78 H118 N8 Nb2 O8, C7 H8'
_chemical_formula_sum            'C85 H126 N8 Nb2 O8'
_chemical_formula_weight         1573.75
_chemical_melting_point          451
_chemical_name_common            '[(BDI)Nb(NtBu)(\m-O2CN(tBu)CO2)]2'
_chemical_name_systematic
'bis(\m2-(tert-butyl)iminodicarboxylato)-bis(tert-butyl)imino-bis(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-diniobium(V) toluene solvate'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-05-13
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-15 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.348(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1406(16)
_cell_length_b                   25.100(3)
_cell_length_c                   22.772(3)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.46
_cell_volume                     9125.0(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.0966
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            71870
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.415
_diffrn_reflns_theta_min         1.257
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6712
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0702 before and 0.0511 after correction.
The Ratio of minimum to maximum transmission is 0.9007.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       plate
_exptl_crystal_F_000             3352
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
TITL bmkxr31_0m in P2(1)/c
CELL   17.1406   25.1000   22.7720     90.00    111.35     90.00
SPGR P21/c
C101 0.189 0.531 0.752 !       6.39 eA-3
C102 0.754 0.382 0.243 !       5.03 eA-3
C103 0.305 0.892 0.297 !       4.78 eA-3
C104 0.258 0.977 0.313 !       4.48 eA-3
C105 0.317 0.563 0.827 !       4.45 eA-3
C106 0.251 0.936 0.290 !       4.29 eA-3
C107 0.821 0.078 0.781 !       4.09 eA-3
C108 0.141 0.891 0.178 !       4.03 eA-3
C109 0.785 0.366 0.273 !       3.89 eA-3
C110 0.530 0.029 0.481 !       3.72 eA-3
C111 0.900 0.411 0.336 !       3.48 eA-3
C112 0.133 0.946 0.184 !       3.46 eA-3
C113 0.596 0.960 0.528 !       2.91 eA-3
C114 0.458 0.494 0.992 !       2.77 eA-3
C115 0.377 0.489 0.000 !       2.01 eA-3
C116 0.328 0.984 0.499 !       1.91 eA-3
C117 0.340 0.026 0.476 !       1.87 eA-3
C118 0.605 0.037 0.480 !       1.83 eA-3
C119 0.721 0.507 0.159 !       1.15 eA-3
C120 0.543 0.581 0.029 !       0.99 eA-3
C121 0.761 0.994 0.671 !       0.97 eA-3
C122 0.640 0.455 0.109 !       0.94 eA-3
Q123 0.663 0.063 0.453 !       0.90 eA-3
C124 0.326 0.932 0.282 !       0.90 eA-3
C125 0.674 0.424 0.121 !       0.89 eA-3
C126 0.920 0.461 0.344 !       0.87 eA-3
C127 0.631 0.037 0.651 !       0.84 eA-3
C128 0.282 0.983 0.461 !       0.83 eA-3
C129 0.871 0.445 0.261 !       0.81 eA-3
C130 0.757 0.473 0.139 !       0.81 eA-3
C131 0.428 0.937 0.475 !       0.80 eA-3
C132 0.564 0.029 0.523 !       0.77 eA-3
Q133 0.706 0.446 0.111 !       0.77 eA-3
C134 0.294 0.643 0.750 !       0.77 eA-3
C135 0.254 0.028 0.454 !       0.76 eA-3
Q136 0.735 0.163 0.693 !       0.75 eA-3
C137 0.401 0.495 0.945 !       0.75 eA-3
C138 0.096 0.572 0.623 !       0.75 eA-3
C139 0.950 0.061 0.828 !       0.75 eA-3
C140 0.835 0.008 0.709 !       0.74 eA-3
C141 0.205 0.637 0.775 !       0.74 eA-3
C142 0.690 0.133 0.659 !       0.73 eA-3
C143 0.062 0.869 0.155 !       0.73 eA-3
C144 0.640 0.087 0.491 !       0.72 eA-3
Q145 0.537 0.571 0.071 !       0.72 eA-3
C146 0.749 0.492 0.048 !       0.71 eA-3
Q147 0.483 0.945 0.459 !       0.70 eA-3
Q148 0.672 0.021 0.463 !       0.70 eA-3
C149 0.165 0.580 0.670 !       0.70 eA-3
C150 0.390 0.568 0.053 !       0.70 eA-3
Q151 0.152 0.733 0.734 !       0.69 eA-3
C152 0.416 0.580 0.046 !       0.69 eA-3
Q153 0.918 0.131 0.726 !       0.69 eA-3
Q154 0.438 0.226 0.492 !       0.69 eA-3
Q155 0.397 0.577 0.884 !       0.69 eA-3
Q156 0.503 0.601 0.083 !       0.68 eA-3
C157 0.475 0.506 0.953 !       0.68 eA-3
Q158 0.624 0.087 0.698 !       0.68 eA-3
Q159 0.568 0.055 0.640 !       0.68 eA-3
Q160 0.717 0.407 0.158 !       0.68 eA-3
C161 0.287 0.069 0.387 !       0.68 eA-3
Q162 0.482 0.111 0.468 !       0.67 eA-3
Q163 0.156 0.086 0.035 !       0.67 eA-3
Q164 0.620 0.956 0.438 !       0.67 eA-3
Q165 0.036 0.554 0.584 !       0.67 eA-3
Q166 0.070 0.460 0.258 !       0.66 eA-3
C167 0.475 0.585 0.037 !       0.65 eA-3
Q168 0.294 0.532 0.773 !       0.65 eA-3
Q169 0.620 0.680 0.345 !       0.65 eA-3
Q170 0.596 0.580 0.002 !       0.65 eA-3
C171 0.661 0.454 0.033 !       0.65 eA-3
Q172 0.026 0.250 0.136 !       0.65 eA-3
Q173 0.382 0.412 0.971 !       0.65 eA-3
Q174 0.753 0.351 0.149 !       0.65 eA-3
C175 0.455 0.530 0.073 !       0.64 eA-3
Q176 0.369 0.546 0.796 !       0.64 eA-3
Q177 0.769 0.635 0.538 !       0.64 eA-3
Q178 0.531 0.030 0.359 !       0.64 eA-3
Q179 0.818 0.041 0.844 !       0.63 eA-3
C180 0.720 0.515 0.074 !       0.63 eA-3
Q181 0.297 0.014 0.313 !       0.63 eA-3
Q182 0.409 0.555 0.115 !       0.63 eA-3
C183 0.211 0.593 0.799 !       0.63 eA-3
Q184 0.036 0.585 0.314 !       0.63 eA-3
Q185 0.737 0.313 0.055 !       0.62 eA-3
Q186 0.145 0.498 0.650 !       0.62 eA-3
Q187 0.555 0.453 0.407 !       0.62 eA-3
C188 0.145 0.970 0.116 !       0.62 eA-3
Q189 0.607 0.219 0.548 !       0.62 eA-3
C190 0.731 0.017 0.593 !       0.62 eA-3
Q191 0.018 0.694 0.329 !       0.62 eA-3
Q192 0.480 0.960 0.426 !       0.61 eA-3
Q193 0.320 0.149 0.139 !       0.61 eA-3
Q194 0.671 0.601 0.128 !       0.61 eA-3
Q195 0.248 0.188 0.219 !       0.61 eA-3
Q196 0.733 0.429 0.117 !       0.61 eA-3
C197 0.384 0.479 0.918 !       0.61 eA-3
Q198 0.302 0.905 0.414 !       0.61 eA-3
C199 0.134 0.834 0.198 !       0.60 eA-3
;
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         16734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0468P)^2^+2.3240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11211
_reflns_number_total             16734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03489d2.cif
_cod_data_source_block           bmkxr31_sq
_cod_original_cell_volume        9125.1(17)
_cod_database_code               1559321
_shelx_shelxl_version_number     2018/3
_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
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C51(H51), C54(H54), C63(H63), C66(H66)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C41(H41),
 C47(H47), C48(H48), C49(H49), C59(H59), C60(H60), C61(H61), C81(H81), C82(H82),
  C83(H83), C84(H84), C85(H85)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C39(H39A,H39B,H39C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C64(H64A,
 H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C),
 C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C76(H76A,H76B,
 H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'