Synthesis and coordination of a hybrid phosphinoferrocene sulfonamide ligand
Varmužová, Věra; Horký, Filip; Štěpnička, Petr; New Journal of Chemistry 45 (2021) 3319–3327; doi:10.1039/D1NJ00080B

data_7060362
_publ_section_title
;
 Synthesis and coordination of a hybrid phosphinoferrocene sulfonamide
 ligand
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3319
_journal_page_last               3327
_journal_paper_doi               10.1039/D1NJ00080B
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C23 H25 B Fe N O2 P S'
_chemical_formula_sum            'C23 H25 B Fe N O2 P S'
_chemical_formula_weight         477.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2020-12-22 deposited with the CCDC.	2021-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.5588(9)
_cell_length_b                   9.0762(4)
_cell_length_c                   51.788(3)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      70.10
_cell_measurement_theta_min      3.41
_cell_volume                     8723.3(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service vV6.2.9'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'PLATON (Spek, 2017)'
_computing_publication_material  'PLATON (Spek, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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_source         'I\mS micro-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            67871
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.220
_diffrn_reflns_theta_min         3.414
_exptl_absorpt_coefficient_mu    7.292
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.28
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       plate
_exptl_crystal_F_000             3968
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 6770 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0078(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1085
_refine_ls_number_reflns         16364
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0354P)^2^+6.9434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                15405
_reflns_number_total             16364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00080b2.cif
_cod_data_source_block           vv11
_cod_depositor_comments
'Adding full bibliography for 7060358--7060363.cif.'
_cod_original_cell_volume        8723.3(7)
_cod_database_code               7060362
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.310
_shelx_estimated_absorpt_t_max   0.811
_shelx_res_checksum              92851