Late-stage ligand functionalization <i>via</i> the Staudinger reaction using phosphine-appended 2,2'-bipyridine.
Taher, Deeb; Wilson, Jessica R.; Ritch, Grayson; Zeller, Matthias; Szymczak, Nathaniel K.; Chemical communications (Cambridge, England) 57 (2021) 5718–5721; doi:10.1039/d1cc01407b

data_7128317
_publ_section_title
;
 Late-stage ligand functionalization <i>via</i> the Staudinger reaction
 using phosphine-appended 2,2'-bipyridine.
;
_journal_issue                   46
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5718
_journal_page_last               5721
_journal_paper_doi               10.1039/d1cc01407b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'C48 H34 Cl F6 Fe N4 P2, F6 P, 1.155(C4 H10 O), 0.734(C2 H3 N)'
_chemical_formula_sum            'C54.09 H47.75 Cl F12 Fe N4.73 O1.16 P3'
_chemical_formula_weight         1194.74
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-03-13 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.1160(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   18.7721(2)
_cell_length_c                   17.1927(2)
_cell_measurement_reflns_used    26681
_cell_measurement_temperature    85(2)
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_cell_measurement_theta_min      3.5260
_cell_volume                     5394.50(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement
;  
SHELXL-2018/3 (Sheldrick, 2015, 2018), 
SHELXLE Rev1005 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device
'Rigaku AFC10K Saturn 944+ CCD-based X-ray diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            81879
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.327
_diffrn_reflns_theta_min         2.643
_diffrn_source                   'Cu-target micro-focus rotating anode'
_diffrn_source_type
'Micromax-007HF (Cu) micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    4.295
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       plate
_exptl_crystal_F_000             2442.6
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         10032
_refine_ls_number_restraints     427
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0681P)^2^+3.3905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9083
_reflns_number_total             10032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01407b2.cif
_cod_data_source_block           gr5174
_cod_depositor_comments
'Adding full bibliography for 7128313--7128317.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7128317
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.605
_shelx_estimated_absorpt_t_max   0.699
_shelx_res_checksum              33239