Reactions of an Anionic Chelate Phosphane/borata-alkene Ligand with [Rh(nbd)Cl]2, [Rh(CO)2Cl]2 and [Ir(cod)Cl]2.
Watanabe, Kohei; Ueno, Atsushi; Tao, Xin; Skoch, Karel; Jie, Xiaoming; Vagin, Sergei; Rieger, Bernhard; Daniliuc, Constantin Gabriel; Letzel, Mathias C.; Kehr, Gerald; Erker, Gerhard; Chemical Science  (2020) –; doi:10.1039/D0SC02223C

data_1558364
_publ_section_title
;
 Reactions of an Anionic Chelate Phosphane/borata-alkene Ligand with
 [Rh(nbd)Cl]2, [Rh(CO)2Cl]2 and [Ir(cod)Cl]2.
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02223C
_journal_year                    2020
_chemical_formula_sum            'C43 H52 B F10 Li N P'
_chemical_formula_weight         821.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           'APEX3 v2016.1-0'
_audit_update_record
;
2019-10-19 deposited with the CCDC.	2020-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                98.0450(10)
_cell_angle_beta                 99.3150(10)
_cell_angle_gamma                111.182(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0597(2)
_cell_length_b                   12.1028(3)
_cell_length_c                   16.2479(5)
_cell_measurement_reflns_used    5314
_cell_measurement_temperature    173.(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     2130.75(10)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection
;

Collect (Nonius B.V., 1998)
;
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'rotating anode Nonius FR591'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19240
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.09
_diffrn_source                   'Mo rotating anode'
_diffrn_source_type              'Mo rotating anode'
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.336
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         7372
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0730
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+3.9006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                5599
_reflns_number_total             7372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02223c2.cif
_cod_data_source_block           erk9302
_cod_database_code               1558364
_shelx_res_checksum              95816