#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2011905.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2011905 loop_ _publ_author_name 'N\"ather, Christian' 'Greve, Jan' _publ_section_title ; Poly[copper(I)-\m-bromo-\m-2,3-dimethylpyrazine-N:N'] ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 377 _journal_page_last 378 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Cu Br (C6 H8 N2)]' _chemical_formula_moiety 'C6 H8 Br Cu N2' _chemical_formula_sum 'C6 H8 Br Cu N2' _chemical_formula_weight 251.59 _chemical_name_systematic ; Poly[copper(I)-\m-bromo-\m-2,3-dimethylpyrazine-N:N'] ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 11.459(2) _cell_length_b 9.7078(11) _cell_length_c 13.468(4) _cell_measurement_reflns_used 140 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 18.5 _cell_measurement_theta_min 12 _cell_volume 1498.2(5) _computing_cell_refinement DIF4 _computing_data_collection 'DIF4 (Stoe & Cie, 1992)' _computing_data_reduction 'REDU4 (Stoe & Cie, 1992)' _computing_molecular_graphics 'XP in SHELXTL/PC (Siemens, 1990)' _computing_publication_material 'CIFTAB in SHELXL97' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .999 _diffrn_measured_fraction_theta_max .999 _diffrn_measurement_device_type 'Phillips PW-1100 four-circle' _diffrn_measurement_method \w-\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .031 _diffrn_reflns_av_sigmaI/netI .0306 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 2821 _diffrn_reflns_theta_full 30.03 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_theta_min 3.02 _diffrn_standards_decay_% none _diffrn_standards_interval_time 120 _diffrn_standards_number 4 _exptl_absorpt_coefficient_mu 8.166 _exptl_absorpt_correction_T_max .520 _exptl_absorpt_correction_T_min .386 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(X-SHAPE (Stoe & Cie, 1998)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular polyhedron' _exptl_crystal_F_000 976 _exptl_crystal_size_max .12 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .08 _refine_diff_density_max .72 _refine_diff_density_min -.87 _refine_ls_extinction_coef .0036(4) _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 94 _refine_ls_number_reflns 2186 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all .057 _refine_ls_R_factor_gt .032 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0467P)^2^+0.6968P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .085 _reflns_number_gt 1681 _reflns_number_total 2186 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file sk1444.cif _[local]_cod_data_source_block I _cod_original_cell_volume 1498.2(6) _cod_database_code 2011905 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Cu1 .46639(3) .57377(4) .60884(3) .03019(13) Uani d . 1 Cu Br1 .50724(3) .68412(3) .44811(2) .02844(11) Uani d . 1 Br N1 .6050(2) .5955(2) .70725(17) .0201(5) Uani d . 1 N C1 .6095(2) .5307(3) .7951(2) .0192(5) Uani d . 1 C C2 .7088(2) .5406(3) .8561(2) .0216(5) Uani d . 1 C N2 .8046(2) .6080(3) .82603(18) .0222(5) Uani d . 1 N C3 .7977(2) .6744(3) .7382(2) .0241(6) Uani d . 1 C H3 .8618 .7242 .7158 .029 Uiso calc R 1 H C4 .6988(2) .6702(3) .6812(2) .0233(6) Uani d . 1 C H4 .6965 .7208 .6225 .028 Uiso calc R 1 H C5 .5068(3) .4461(3) .8250(2) .0278(6) Uani d . 1 C H5A .4592 .4977 .8704 .042 Uiso calc R 1 H H5B .5333 .3632 .8568 .042 Uiso calc R 1 H H5C .4619 .4229 .7672 .042 Uiso calc R 1 H C6 .7101(3) .4799(4) .9578(2) .0367(8) Uani d . 1 C H6A .7739 .5181 .9949 .055 Uiso calc R 1 H H6B .7193 .3818 .9531 .055 Uiso calc R 1 H H6C .6380 .5007 .9907 .055 Uiso calc R 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1 .0243(2) .0399(2) .0264(2) -.00295(16) -.00025(14) .00090(17) Br1 .0405(2) .02242(16) .02244(16) .00252(12) -.00023(11) .00262(11) N1 .0193(10) .0217(11) .0193(10) -.0010(9) -.0025(8) .0012(9) C1 .0190(12) .0170(12) .0217(12) .0023(10) .0027(10) .0019(10) C2 .0194(13) .0246(13) .0208(12) .0025(11) .0013(9) .0010(11) N2 .0163(11) .0282(12) .0221(11) -.0002(9) .0003(8) .0009(10) C3 .0219(13) .0269(14) .0235(13) -.0052(11) .0023(10) .0037(12) C4 .0257(14) .0245(13) .0197(12) -.0022(11) -.0001(10) .0047(11) C5 .0234(13) .0291(14) .0309(14) -.0041(11) .0028(12) .0071(13) C6 .0268(15) .060(2) .0234(15) -.0011(16) .0003(11) .0159(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu .3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 Cu1 N1 6_557 . 113.34(10) y N2 Cu1 Br1 6_557 . 118.14(7) y N1 Cu1 Br1 . . 111.79(7) y N2 Cu1 Br1 6_557 5_666 112.15(7) y N1 Cu1 Br1 . 5_666 101.21(7) y Br1 Cu1 Br1 . 5_666 97.80(2) y Cu1 Br1 Cu1 . 5_666 82.20(2) y C1 N1 C4 . . 117.0(2) n C1 N1 Cu1 . . 122.95(18) n C4 N1 Cu1 . . 119.96(19) n N1 C1 C2 . . 121.0(2) n N1 C1 C5 . . 117.8(2) n C2 C1 C5 . . 121.2(2) n N2 C2 C1 . . 121.3(3) n N2 C2 C6 . . 117.5(3) n C1 C2 C6 . . 121.2(3) n C2 N2 C3 . . 116.7(2) n C2 N2 Cu1 . 6_657 121.68(19) y C3 N2 Cu1 . 6_657 119.93(19) y N2 C3 C4 . . 121.8(3) n N2 C3 H3 . . 119.1 n C4 C3 H3 . . 119.1 n N1 C4 C3 . . 122.1(3) n N1 C4 H4 . . 119 n C3 C4 H4 . . 119 n C1 C5 H5A . . 110 n C1 C5 H5B . . 110 n H5A C5 H5B . . 110 n C1 C5 H5C . . 110 n H5A C5 H5C . . 110 n H5B C5 H5C . . 110 n C2 C6 H6A . . 110 n C2 C6 H6B . . 110 n H6A C6 H6B . . 110 n C2 C6 H6C . . 110 n H6A C6 H6C . . 110 n H6B C6 H6C . . 110 n loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 N2 6_557 2.077(2) y Cu1 N1 . 2.080(2) y Cu1 Br1 . 2.4602(7) y Cu1 Br1 5_666 2.6358(6) y Br1 Cu1 5_666 2.6358(6) n N1 C1 . 1.341(3) n N1 C4 . 1.343(4) n C1 C2 . 1.407(4) n C1 C5 . 1.491(4) n C2 N2 . 1.341(4) n C2 C6 . 1.491(4) n N2 C3 . 1.349(4) n N2 Cu1 6_657 2.077(2) n C3 C4 . 1.370(4) n C3 H3 . .93 n C4 H4 . .93 n C5 H5A . .96 n C5 H5B . .96 n C5 H5C . .96 n C6 H6A . .96 n C6 H6B . .96 n C6 H6C . .96 n