Competitive Activation of N−C and C−H Bonds of the PNP Framework by Monovalent Rhodium and Iridium
Weng, Wei; Guo, Chengyun; Moura, Claudia; Yang, Lin; Foxman, Bruce M.; Ozerov, Oleg V.; Organometallics 24 (2005) 3487–; doi:10.1021/om050346o

data_4075953
_publ_section_title
;
 Competitive Activation of N&#x2212;C and C&#x2212;H Bonds of the PNP
 Framework by Monovalent Rhodium and Iridium
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3487
_journal_paper_doi               10.1021/om050346o
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C27 H39 Br2 N1 P2'
_chemical_formula_sum            'C27 H39 Br2 N P2'
_chemical_formula_weight         599.37
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             04-12-14
_audit_creation_method           CRYSTALS_ver_12.51
_cell_angle_alpha                90
_cell_angle_beta                 90.269(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.651(3)
_cell_length_b                   8.2918(12)
_cell_length_c                   20.935(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      45
_cell_measurement_theta_min      21
_cell_volume                     2890.4(8)
_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      294
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.011
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6063
_diffrn_reflns_theta_full        74.165
_diffrn_reflns_theta_max         74.165
_diffrn_reflns_theta_min         2.654
_diffrn_standards_decay_%        16.30
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.703
_exptl_absorpt_correction_T_max  0.51
_exptl_absorpt_correction_T_min  0.20
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 
 Azimutal absorption correction (North et al., 1968) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.61
_refine_ls_extinction_coef       37(6)
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0430
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3855
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.000999
_refine_ls_structure_factor_coef F
_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: 
 2.72 2.08 1.91 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1386
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0701
_reflns_limit_h_max              20
_reflns_limit_h_min              0
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              -26
_reflns_number_gt                3855
_reflns_number_total             5888
_reflns_threshold_expression     I>1.96u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.6241(18)
_oxford_structure_analysis_title OZ017B
_cod_data_source_file            om050346osi20050503_044401.cif
_cod_data_source_block           Compound1d_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C27 H39 Br2 N1 P2'
_cod_database_code               4075953