Online Monitoring of Hydroformylation Intermediates by ESI-MS
Beierlein, Christian H.; Breit, Bernhard; Paz Schmidt, Roberto A.; Plattner, Dietmar A.; Organometallics 29 (2010) 2521–; doi:10.1021/om100131t

data_4065798
_publ_section_title
;
 Online Monitoring of Hydroformylation Intermediates by ESI-MS
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2521
_journal_paper_doi               10.1021/om100131t
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C42 H39 N2 O2 P2 Rh, C H2 Cl2'
_chemical_formula_sum            'C43 H41 Cl2 N2 O2 P2 Rh'
_chemical_formula_weight         853.53
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.8347(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5843(4)
_cell_length_b                   20.4005(5)
_cell_length_c                   16.7757(5)
_cell_measurement_reflns_used    15877
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3906.3(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'long-fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0787
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27443
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         8941
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+1.5123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1198
_reflns_number_gt                5983
_reflns_number_total             8941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100131t_si_001.cif
_cod_data_source_block           jg008
_cod_original_sg_symbol_H-M      'P 2(1)/n'
_cod_database_code               4065798