One-step synthesis of alkenyl ketone complexes from Cp*RhCl2(PPh3), alkyne and H2O in the presence of KPF6
Ogata, Kenichi; Kuge, Katsuaki; Tatsumi, Kazuyuki; Yamamoto, Yasuhiro; Chemical Communications  (2002) 128–; doi:10.1039/b108953f

data_7114090
_publ_section_title
;
 One-step synthesis of alkenyl ketone complexes from Cp*RhCl2(PPh3),
 alkyne and H2O in the presence of KPF6
;
_journal_issue                   2
_journal_name_full               'Chemical Communications'
_journal_page_first              128
_journal_paper_doi               10.1039/b108953f
_journal_year                    2002
_chemical_formula_sum            'C46 H47 F6 O P2 Rh'
_chemical_formula_weight         894.72
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_cell_angle_alpha                90
_cell_angle_beta                 103.06(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.363(8)
_cell_length_b                   9.32(1)
_cell_length_c                   20.289(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    301.2
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      12.2
_cell_volume                     2093(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    'DIRDIF94 (PATTY)'
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9992
_diffrn_measurement_device_type  'Rigaku AFC5S'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            4145
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_standards_decay_%        0.28
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.98
_refine_diff_density_min         -1.04
_refine_ls_abs_structure_Flack   0.17(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.336
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     476
_refine_ls_number_reflns         3676
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.0566
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1803
_reflns_number_gt                3285
_reflns_number_total             3690
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            b108953f.txt
_cod_data_source_block           afc5s.xtl_master_file
_cod_original_cell_volume        2093(2)
_cod_original_formula_sum        'C46 H47 F6 O P2 Rh '
_cod_database_code               7114090