Dimethyl 2,2'-bipyridine-6,6'-dicarboxylate and bis(dimethyl 2,2'-bipyridine-6,6'-dicarboxylato-κ^2^<i>N</i>,<i>N</i>')copper(I) tetrafluoroborate
Alexander J. Blake; Neil R. Champness; Pamela V. Mason; Claire Wilson; Acta Crystallographica Section C 63 (2007) m280–m282; doi:10.1107/S0108270107020914

data_2015994
_publ_section_title
;
 Dimethyl 2,2'-bipyridine-6,6'-dicarboxylate and bis(dimethyl
 2,2'-bipyridine-6,6'-dicarboxylato-\k^2^<i>N</i>,<i>N</i>')copper(I)
 tetrafluoroborate
;
_journal_coeditor_code           HJ3036
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m280
_journal_page_last               m282
_journal_paper_doi               10.1107/S0108270107020914
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C14 H12 N2 O4'
_chemical_formula_moiety         'C14 H12 N2 O4'
_chemical_formula_sum            'C14 H12 N2 O4'
_chemical_formula_weight         272.26
_chemical_name_systematic
;
Dimethyl 2,2'-bipyridine-6,6'-dicarboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 109.448(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4182(15)
_cell_length_b                   6.8889(11)
_cell_length_c                   9.7931(15)
_cell_measurement_reflns_used    1954
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     599.13(16)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT and SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material
'enCIFer (Allen <i>et al.</i>,  2004) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_av_sigmaI/netI    0.039
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3716
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.61
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.22
_refine_ls_extinction_coef       0.015(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.13
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.13
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0629P)^2^+0.0616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.109
_refine_ls_wR_factor_ref         0.113
_reflns_number_gt                1167
_reflns_number_total             1360
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hj3036.cif
_cod_data_source_block           I
_cod_original_cell_volume        599.1(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2015994