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_1558368
_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            'C44 H27 B2 F20 P'
_chemical_formula_weight         988.24
_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                101.416(2)
_cell_angle_beta                 99.845(2)
_cell_angle_gamma                98.080(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4373(3)
_cell_length_b                   11.5018(3)
_cell_length_c                   20.0520(6)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    104.(2)
_cell_measurement_theta_max      68.3295
_cell_measurement_theta_min      4.1238
_cell_volume                     2286.61(12)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection
;

APEX3 v2016.1-0 (Bruker AXS Inc., 2016)
;
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_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      104.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'MX mirror'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24980
_diffrn_reflns_theta_full        68.40
_diffrn_reflns_theta_max         68.40
_diffrn_reflns_theta_min         4.12
_diffrn_source                   'Cu ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    1.565
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Bruker AXS (2014). SADABS, Version 2014/5, Bruker AXS Inc., Madison, Wisconsin,
USA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.196
_refine_diff_density_min         -0.421
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         8162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0487P)^2^+1.9349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1157
_reflns_number_gt                6547
_reflns_number_total             8162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02223c2.cif
_cod_data_source_block           erk8821
_cod_original_cell_volume        2286.61(11)
_cod_database_code               1558368
_shelx_res_checksum              81890
_shelx_fab_checksum              249