Convergent (De)Hydrogenative Pathways via a Rhodium α-Hydroxylalkyl Complex
Sung, Simon; Boon, Jie Kang; Lee, Johnathan J. C.; Rajabi, Nasir A.; Macgregor, Stuart A.; Krämer, Tobias; Young, Rowan D.; Organometallics 36 (2017) 1609–; doi:10.1021/acs.organomet.7b00158

data_4087278
_publ_section_title
;
 Convergent (De)Hydrogenative Pathways via a Rhodium \a-Hydroxylalkyl
 Complex
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1609
_journal_paper_doi               10.1021/acs.organomet.7b00158
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C55 H44 O1 P3 Rh1'
_chemical_formula_sum            'C55 H44 O P3 Rh'
_chemical_formula_weight         916.78
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 109.692(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8773(11)
_cell_length_b                   19.4837(15)
_cell_length_c                   18.3485(13)
_cell_measurement_reflns_used    73511
_cell_measurement_temperature    150
_cell_measurement_theta_max      50
_cell_measurement_theta_min      0.001
_cell_volume                     4334.4(6)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.092
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            74023
_diffrn_reflns_theta_full        24.760
_diffrn_reflns_theta_max         24.760
_diffrn_reflns_theta_min         2.358
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.34
_refine_diff_density_min         -2.55
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9679
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         7372
_refine_ls_number_restraints     494
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.0868
_refine_ls_shift/su_max          0.0004713
_refine_ls_shift/su_mean         0.0000138
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ +67.15P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2104
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.2096
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                4999
_reflns_number_total             7412
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.76
_oxford_diffrn_Wilson_scale      29.50
_oxford_refine_ls_r_factor_ref   0.1327
_oxford_refine_ls_scale          0.2068(2)
_oxford_reflns_number_all        7378
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            om7b00158_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        4334.4(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C55 H44 O1 P3 Rh1'
_cod_database_code               4087278