Cyclobutadiene Arene Complexes of Rhodium and Iridium
Shvydkiy, Nikita V.; Trifonova, Evgeniya A.; Shved, Andrei M.; Nelyubina, Yulia V.; Chusov, Denis; Perekalin, Dmitry S.; Kudinov, Alexander R.; Organometallics 35 (2016) 3025–; doi:10.1021/acs.organomet.6b00539

data_4088900
_publ_section_title
;
 Cyclobutadiene Arene Complexes of Rhodium and Iridium
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3025
_journal_paper_doi               10.1021/acs.organomet.6b00539
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C16 H26 Rh, F2 O2 P'
_chemical_formula_sum            'C16 H26 F2 O2 P Rh'
_chemical_formula_weight         422.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3540(13)
_cell_length_b                   9.2101(15)
_cell_length_c                   21.622(3)
_cell_measurement_reflns_used    2606
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1663.6(4)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'APEX2 (Bruker, 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX2 DUO CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19126
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.995
_diffrn_reflns_theta_min         1.884
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.983
_refine_diff_density_min         -1.824
_refine_diff_density_rms         0.158
_refine_ls_abs_structure_details
;
 Flack x determined using 1358 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.08(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0899P)^2^+2.6754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3512
_reflns_number_total             4001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00539_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        1663.6(5)
_cod_database_code               4088900
_shelx_estimated_absorpt_t_min   0.690
_shelx_estimated_absorpt_t_max   0.945
_shelxl_version_number           2014/6
_shelx_res_checksum              75213
_shelx_hkl_checksum              29445