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_7128313
_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
'C58 H58 B2 Cl Fe N4 O4 P2, F6 P, 1.397(C4 H10 O), 0.74(C H2 Cl2)'
_chemical_formula_sum            'C64.33 H73.45 B2 Cl2.48 F6 Fe N4 O5.4 P3'
_chemical_formula_weight         1361.28
_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                 110.277(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.1444(16)
_cell_length_b                   18.7701(9)
_cell_length_c                   17.1873(8)
_cell_measurement_reflns_used    8967
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.5979
_cell_measurement_theta_min      2.5267
_cell_volume                     7003.8(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Apex3 v2019.1-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_structure_refinement
;  
SHELXL-2018/3 (Sheldrick, 2015, 2018), 
SHELXLE Rev1117 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type
;
Bruker AXS D8 Quest diffractometer with PhotonII charge-integrating pixel 
array detector (CPAD)
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1130
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            114702
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.600
_diffrn_reflns_theta_min         2.364
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.
(2015). J. Appl. Cryst. 48, 3-10.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       plate
_exptl_crystal_F_000             2831
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.152
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1152
_refine_ls_number_reflns         21068
_refine_ls_number_restraints     1146
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1219
_refine_ls_R_factor_gt           0.0672
_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^)+(0.1112P)^2^+4.0277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.2202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12382
_reflns_number_total             21068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01407b2.cif
_cod_data_source_block           DeebTaher115_0m
_cod_depositor_comments
'Adding full bibliography for 7128313--7128317.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C64.33 H73.45 B2 Cl2.48 F6 Fe N4 O5.40 P3'
_cod_database_code               7128313
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.860
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              30271