Synthesis of Bis(phosphine) and N-Heterocyclic Carbene Supported α- Diazoalkyl Complexes of Copper(I)
Iluc, Vlad M.; Laskowski, Carl A.; Hillhouse, Gregory L.; Organometallics 28 (2009) 6135–; doi:10.1021/om900566k

data_4070010
_publ_section_title
;
 Synthesis of Bis(phosphine) and N-Heterocyclic Carbene Supported \a-
 Diazoalkyl Complexes of Copper(I)
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              6135
_journal_paper_doi               10.1021/om900566k
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C47 H75 Cu N2 P2'
_chemical_formula_weight         793.57
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.591(16)
_cell_angle_beta                 88.795(14)
_cell_angle_gamma                79.616(2)
_cell_formula_units_Z            4
_cell_length_a                   14.2743(13)
_cell_length_b                   15.4477(14)
_cell_length_c                   21.019(2)
_cell_measurement_reflns_used    93
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.36
_cell_volume                     4557.9(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.1268
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22738
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.9689
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Norton et al.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         15818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                10151
_reflns_number_total             15818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900566k_si_001.cif
_cod_data_source_block           (dtbpe)Cu[N(nBu)NCH(dmp)]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4070010