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_4087277
_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         'C58 H47 O1 P3 Rh1'
_chemical_formula_sum            'C58 H47 O P3 Rh'
_chemical_formula_weight         955.84
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                70.865(5)
_cell_angle_beta                 78.917(5)
_cell_angle_gamma                64.645(5)
_cell_formula_units_Z            2
_cell_length_a                   11.6113(14)
_cell_length_b                   12.6370(15)
_cell_length_c                   18.201(2)
_cell_measurement_reflns_used    84637
_cell_measurement_temperature    150
_cell_measurement_theta_max      55
_cell_measurement_theta_min      0.01
_cell_volume                     2275.9(5)
_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 0.994
_diffrn_measured_fraction_theta_max 0.987
_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  0.057
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            84637
_diffrn_reflns_theta_full        26.512
_diffrn_reflns_theta_max         27.617
_diffrn_reflns_theta_min         2.339
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Dark green'
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             986
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.31
_refine_diff_density_min         -2.00
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         10376
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1541
_refine_ls_R_factor_gt           0.1396
_refine_ls_shift/su_max          0.0001506
_refine_ls_shift/su_mean         0.0000062
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 7.65 8.19 2.20 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3332
_refine_ls_wR_factor_gt          0.3308
_refine_ls_wR_factor_ref         0.3332
_reflns_limit_h_max              15
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                8625
_reflns_number_total             10428
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.92
_oxford_diffrn_Wilson_scale      57.26
_oxford_refine_ls_r_factor_ref   0.1540
_oxford_refine_ls_scale          0.1652(3)
_oxford_reflns_number_all        10380
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            om7b00158_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        2275.9(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C58 H47 O1 P3 Rh1'
_cod_database_code               4087277