#------------------------------------------------------------------------------
#$Date: 2017-05-20 04:57:54 +0300 (Sat, 20 May 2017) $
#$Revision: 196814 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/30/7043051.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7043051
loop_
_publ_author_name
'Vaid, Thomas'
'Kelley, Steven Paul'
'Rogers, Robin D.'
_publ_section_title
;
 Metal Carbonate Complexes Formed Through the Capture of Ambient O2 and
 CO2 by Elemental Metals in 1-methylimidazole: Molecular Cu(CO3)(MeIm)3
 and Polymeric M(CO3)(MeIm)2·2H2O (M = Co, Zn)
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01787A
_journal_year                    2017
_chemical_formula_sum            'C13 H18 Cu N6 O3'
_chemical_formula_weight         369.87
_chemical_name_systematic        Cu(CO3)(1-methylimidazole)3
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-10-20 deposited with the CCDC.
2017-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.292(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.232(4)
_cell_length_b                   8.981(3)
_cell_length_c                   13.232(4)
_cell_measurement_reflns_used    7828
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.58
_cell_measurement_theta_min      2.75
_cell_volume                     1569.9(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20773
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         2.742
_exptl_absorpt_coefficient_mu    1.416
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             764
_exptl_crystal_recrystallization_method 'crystallization during formation'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
; 
 Flack x determined using 1573 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.002(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3594
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0277P)²+1.0692P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0628
_reflns_Friedel_coverage         0.987
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                3373
_reflns_number_total             3594
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt01787a2.cif
_cod_data_source_block           s1
_cod_original_cell_volume        1569.9(8)
_cod_database_code               7043051
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.871
_shelx_estimated_absorpt_t_max   0.946
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cu Cu 0.12670(3) -0.10515(4) 0.37175(3) 0.01776(11) Uani 1 1 d . .
O1 O 0.2101(2) -0.1922(4) 0.2685(2) 0.0321(7) Uani 1 1 d . .
O2 O 0.04616(19) -0.1875(3) 0.2525(2) 0.0268(6) Uani 1 1 d . .
O3 O 0.1328(2) -0.2873(3) 0.12716(18) 0.0269(6) Uani 1 1 d . .
N1 N 0.0093(2) -0.1079(3) 0.4625(2) 0.0194(6) Uani 1 1 d . .
N3 N -0.0883(2) -0.0913(3) 0.5917(2) 0.0221(7) Uani 1 1 d . .
N7 N 0.2391(2) -0.1093(3) 0.4803(2) 0.0202(6) Uani 1 1 d . .
N9 N 0.3509(2) -0.0591(4) 0.6053(2) 0.0202(6) Uani 1 1 d . .
N13 N 0.1268(3) 0.1387(3) 0.3416(2) 0.0218(7) Uani 1 1 d . .
N15 N 0.0986(2) 0.3768(3) 0.3748(3) 0.0228(7) Uani 1 1 d . .
C2 C 0.0058(3) -0.0736(4) 0.5598(3) 0.0208(8) Uani 1 1 d . .
H2 H 0.0623 -0.0409 0.6015 0.025 Uiso 1 1 calc R U
C4 C -0.1491(3) -0.1360(4) 0.5108(3) 0.0243(8) Uani 1 1 d . .
H4 H -0.2197 -0.1558 0.5100 0.029 Uiso 1 1 calc R U
C5 C -0.0884(3) -0.1467(4) 0.4309(3) 0.0219(8) Uani 1 1 d . .
H5 H -0.1100 -0.1762 0.3641 0.026 Uiso 1 1 calc R U
C6 C -0.1202(3) -0.0622(5) 0.6946(3) 0.0294(9) Uani 1 1 d . .
H6A H -0.1486 0.0383 0.6977 0.044 Uiso 1 1 calc R U
H6B H -0.0616 -0.0705 0.7430 0.044 Uiso 1 1 calc R U
H6C H -0.1717 -0.1352 0.7116 0.044 Uiso 1 1 calc R U
C8 C 0.2682(3) -0.0105(4) 0.5501(3) 0.0192(7) Uani 1 1 d . .
H8 H 0.2355 0.0821 0.5602 0.023 Uiso 1 1 calc R U
C10 C 0.3758(3) -0.1964(5) 0.5686(3) 0.0251(8) Uani 1 1 d . .
H10 H 0.4305 -0.2579 0.5924 0.030 Uiso 1 1 calc R U
C11 C 0.3068(3) -0.2267(4) 0.4920(3) 0.0265(8) Uani 1 1 d . .
H11 H 0.3050 -0.3150 0.4523 0.032 Uiso 1 1 calc R U
C12 C 0.4071(3) 0.0203(5) 0.6871(3) 0.0331(10) Uani 1 1 d . .
H12A H 0.3596 0.0739 0.7281 0.050 Uiso 1 1 calc R U
H12B H 0.4537 0.0914 0.6583 0.050 Uiso 1 1 calc R U
H12C H 0.4457 -0.0513 0.7299 0.050 Uiso 1 1 calc R U
C14 C 0.0858(3) 0.2330(4) 0.4028(3) 0.0223(8) Uani 1 1 d . .
H14 H 0.0510 0.2039 0.4604 0.027 Uiso 1 1 calc R U
C16 C 0.1510(3) 0.3719(4) 0.2885(3) 0.0274(9) Uani 1 1 d . .
H16 H 0.1711 0.4546 0.2497 0.033 Uiso 1 1 calc R U
C17 C 0.1687(3) 0.2264(5) 0.2694(3) 0.0268(8) Uani 1 1 d . .
H17 H 0.2047 0.1902 0.2144 0.032 Uiso 1 1 calc R U
C18 C 0.0646(4) 0.5067(4) 0.4297(3) 0.0347(10) Uani 1 1 d . .
H18A H 0.0997 0.5100 0.4969 0.052 Uiso 1 1 calc R U
H18B H -0.0086 0.5000 0.4368 0.052 Uiso 1 1 calc R U
H18C H 0.0799 0.5973 0.3922 0.052 Uiso 1 1 calc R U
C19 C 0.1298(3) -0.2265(4) 0.2109(3) 0.0177(7) Uani 1 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
O1 Cu O2 66.35(11)
O1 Cu N7 93.86(12)
O2 Cu N7 154.03(12)
O1 Cu N1 152.94(13)
O2 Cu N1 94.09(11)
N7 Cu N1 97.95(13)
O1 Cu N13 105.08(13)
O2 Cu N13 103.23(12)
N7 Cu N13 97.97(12)
N1 Cu N13 97.30(12)
O1 Cu C19 33.12(12)
O2 Cu C19 33.23(11)
N7 Cu C19 125.29(12)
N1 Cu C19 125.21(12)
N13 Cu C19 106.76(11)
C19 O1 Cu 91.7(2)
C19 O2 Cu 90.4(2)
C2 N1 C5 105.6(3)
C2 N1 Cu 130.2(3)
C5 N1 Cu 124.2(2)
C2 N3 C4 107.7(3)
C2 N3 C6 126.0(3)
C4 N3 C6 126.2(3)
C8 N7 C11 105.7(3)
C8 N7 Cu 131.4(3)
C11 N7 Cu 122.8(2)
C8 N9 C10 107.6(3)
C8 N9 C12 127.1(3)
C10 N9 C12 125.3(3)
C14 N13 C17 104.8(3)
C14 N13 Cu 121.4(2)
C17 N13 Cu 133.7(2)
C14 N15 C16 105.9(3)
C14 N15 C18 125.3(3)
C16 N15 C18 128.7(3)
N1 C2 N3 111.1(3)
N3 C4 C5 106.3(3)
C4 C5 N1 109.2(3)
N7 C8 N9 110.8(3)
C11 C10 N9 106.3(3)
C10 C11 N7 109.6(3)
N13 C14 N15 112.6(3)
C17 C16 N15 106.7(3)
C16 C17 N13 109.9(3)
O3 C19 O1 124.0(3)
O3 C19 O2 124.4(3)
O1 C19 O2 111.6(3)
O3 C19 Cu 178.7(3)
O1 C19 Cu 55.18(17)
O2 C19 Cu 56.42(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cu O1 1.966(3)
Cu O2 1.995(3)
Cu N7 2.007(3)
Cu N1 2.018(3)
Cu N13 2.226(3)
Cu C19 2.394(4)
O1 C19 1.309(5)
O2 C19 1.312(4)
O3 C19 1.237(4)
N1 C2 1.327(5)
N1 C5 1.380(5)
N3 C2 1.347(5)
N3 C4 1.363(5)
N3 C6 1.472(5)
N7 C8 1.323(5)
N7 C11 1.387(5)
N9 C8 1.352(5)
N9 C10 1.372(5)
N9 C12 1.463(5)
N13 C14 1.311(5)
N13 C17 1.379(5)
N15 C14 1.356(5)
N15 C16 1.370(5)
N15 C18 1.459(5)
C4 C5 1.368(5)
C10 C11 1.352(6)
C16 C17 1.354(6)
