Synthesis and properties of 1,2,3-diazapnictol-5-yl substituted ferrocenes
Kozáček, Pavel; Dostál, Libor; Hejda, Martin; Mikysek, Tomáš; R°užička, Aleš; Erben, Milan; New Journal of Chemistry 45 (2021) 18171–18182; doi:10.1039/D1NJ02666F

data_7060917
_publ_section_title
;
 Synthesis and properties of 1,2,3-diazapnictol-5-yl substituted
 ferrocenes
;
_journal_issue                   38
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18171
_journal_page_last               18182
_journal_paper_doi               10.1039/D1NJ02666F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_sum            'C30 H36 Fe2 N2'
_chemical_formula_weight         536.31
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-01-04 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.888(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.5627(10)
_cell_length_b                   10.1352(14)
_cell_length_c                   16.263(2)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.62
_cell_measurement_theta_min      2.38
_cell_volume                     1231.6(3)
_computing_cell_refinement       'APEX3 v2018.1-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1276
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29953
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.376
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.200
_exptl_absorpt_correction_T_max  0.7677
_exptl_absorpt_correction_T_min  0.6166
_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    1.446
_exptl_crystal_description       prism
_exptl_crystal_F_000             564
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.568
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.125
_refine_diff_density_max         1.997
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2937
_refine_ls_number_restraints     225
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0835
_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^)+(0.1329P)^2^+9.6423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2367
_refine_ls_wR_factor_ref         0.2450
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2560
_reflns_number_total             2937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj02666f2.cif
_cod_data_source_block           me190729Fe1
_cod_depositor_comments
'Adding full bibliography for 7060916--7060926.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7060917
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.549
_shelx_estimated_absorpt_t_max   0.865
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.803
;
_shelx_res_checksum              41954