A Niobium Pentafulvene Ethylene Complex: Synthesis, Properties and Reaction Pathways
de Graaff, Simon; Schwitalla, Kevin; Haaker, Carolin Viola; Bengen, Nina; Schmidtmann, Marc; Beckhaus, Ruediger; Dalton Transactions  (2022) –; doi:10.1039/D2DT02063G

data_7710801
_publ_section_title
;
 A Niobium Pentafulvene Ethylene Complex: Synthesis, Properties and
 Reaction Pathways
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02063G
_journal_year                    2022
_chemical_formula_structural     'NbO(C2H5)(C20H19)2 *~0.67C6H14'
_chemical_formula_sum            'C46 H52.33 Nb O'
_chemical_formula_weight         714.11
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-06-21 deposited with the CCDC.	2022-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.554(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9136(15)
_cell_length_b                   6.3645(5)
_cell_length_c                   32.438(3)
_cell_measurement_reflns_used    9076
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.80
_cell_measurement_theta_min      3.97
_cell_volume                     3838.7(6)
_computing_cell_refinement       'Bruker SAINT V8.40A'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT V8.40A'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Photon III CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            70482
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.495
_diffrn_reflns_theta_min         2.376
_diffrn_source                   'I\mS microfocus'
_exptl_absorpt_coefficient_mu    2.790
_exptl_absorpt_correction_T_max  0.8290
_exptl_absorpt_correction_T_min  0.6517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       plate
_exptl_crystal_F_000             1509
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.903
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         7828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7319
_reflns_number_total             7828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02063g2.cif
_cod_data_source_block           3
_cod_original_cell_volume        3838.7(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7710801
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.731
_shelx_estimated_absorpt_t_max   0.897
_shelx_res_checksum              60211
_shelx_hkl_checksum              89485
_shelx_fab_checksum              95423