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_7710804
_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     'NbCl(C20H19)2(C8H9N) *0.5C6H14'
_chemical_formula_sum            'C51 H54 Cl N Nb'
_chemical_formula_weight         809.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.5460(4)
_cell_length_b                   22.2303(7)
_cell_length_c                   25.7237(9)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      2.30
_cell_volume                     8318.1(5)
_computing_cell_refinement       'Bruker SAINT V8.40B'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT V8.40B'
_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 1.000
_diffrn_measurement_device_type  'Bruker Photon III CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            247663
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         1.583
_diffrn_source                   'I\mS microfocus'
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       rod
_exptl_crystal_F_000             3400
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         10738
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0200P)^2^+14.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9076
_reflns_number_total             10738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02063g2.cif
_cod_data_source_block           6
_cod_database_code               7710804
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.955
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              84251
_shelx_hkl_checksum              26065