Benz[e]indenyl and benz[f]indenyl molybdenum compounds: evidence of the η3-coordination mode
Štěpán, Jiří; Vinklárek, Jaromír; Císařová, Ivana; Dostál, Libor; Honzíček, Jan; New Journal of Chemistry 47 (2023) 21396–21403; doi:10.1039/D3NJ04406H

data_7062849
_publ_section_title
;
 Benz[e]indenyl and benz[f]indenyl molybdenum compounds: evidence of the
 \h3-coordination mode
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              21396
_journal_page_last               21403
_journal_paper_doi               10.1039/D3NJ04406H
_journal_volume                  47
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C18 H14 Mo O2'
_chemical_formula_sum            'C18 H14 Mo O2'
_chemical_formula_weight         358.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-09-19 deposited with the CCDC.	2023-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.3280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.1572(3)
_cell_length_b                   6.9602(3)
_cell_length_c                   12.5929(5)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4947
_cell_measurement_theta_min      3.2409
_cell_volume                     713.77(5)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 0.996
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_diffrn_reflns_limit_h_max       10
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_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14824
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         2.501
_diffrn_source                   'I\mS  micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       prism
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.58(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3247
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0164
_refine_ls_R_factor_gt           0.0160
_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^)+(0.0254P)^2^+0.1420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0402
_refine_ls_wR_factor_ref         0.0404
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                3209
_reflns_number_total             3247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04406h2.cif
_cod_data_source_block           mo_jv160930mo1_vinklarek
_cod_depositor_comments
'Adding full bibliography for 7062849--7062851.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7062849
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.805
_shelx_estimated_absorpt_t_max   0.910
_shelx_res_checksum              60504