Olefin coordination in copper(I) complexes of bis(2-pyridyl)amine
Allen, John J.; Barron, Andrew R.; Dalton Transactions  (2009) 878–890; doi:10.1039/b814829e

data_7000390
_publ_section_title
;
 Olefin coordination in copper(I) complexes of bis(2-pyridyl)amine
;
_journal_issue                   5
_journal_name_full               'Dalton Transactions'
_journal_page_first              878
_journal_page_last               890
_journal_paper_doi               10.1039/b814829e
_journal_year                    2009
_chemical_formula_moiety         'C18 H21 Cu N3, B F4'
_chemical_formula_sum            'C18 H21 B Cu F4 N3'
_chemical_formula_weight         429.73
_chemical_melting_point          455
_chemical_name_common
;(2,2'-dipyridylamine)(eta4-1,5-cyclooctadiene)copper(i)
tetrafluoroborate
;
_chemical_name_systematic
'(2,2'-dipyridylamine)(\h4-1,5-cyclooctadiene)copper(I) tetrafluoroborate'
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.30(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.2165(14)
_cell_length_b                   11.797(2)
_cell_length_c                   10.771(2)
_cell_measurement_reflns_used    2043
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.23
_cell_measurement_theta_min      2.57
_cell_volume                     913.0(3)
_computing_cell_refinement       'SMART v5.630 (Bruker-AXS 2003)'
_computing_data_collection       'SMART v5.630 (Bruker-AXS 2003)'
_computing_data_reduction        'Bruker SAINT+ v6.45 (Bruker-AXS 2003)'
_computing_molecular_graphics    'SHELXTL v5.1'
_computing_publication_material  'SHELXTL v5.1'
_computing_structure_refinement  'SHELXTL v5.1'
_computing_structure_solution    'SHELXTL v5.1 (Bruker-AXS, 1998)'
_diffrn_ambient_pressure         101.33
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7472
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.90
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART CCD'
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_T_max  0.7848
_exptl_absorpt_correction_T_min  0.7123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.10 (Bruker-AXS, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             440
_exptl_crystal_recrystallization_method
'cooled sat. soln in MeOH to -12 deg. C for several days'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.456
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.034(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0977P)^2^+1.5308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.1990
_reflns_number_gt                1699
_reflns_number_total             2289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b814829e.txt
_cod_data_source_block           dpacod
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7000390