#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:38:19 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224534 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/90/7049035.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_7049035
loop_
_publ_author_name
'Sapianik, Aleksandr A.'
'Kiskin, Mikhail A.'
'Kovalenko, Konstantin A.'
'Samsonenko, Denis G.'
'Dybtsev, Danil N.'
'Audebrand, Nathalie'
'Sun, Yaguang'
'Fedin, Vladimir P.'
_publ_section_title
;
 Rational synthesis and dimensionality tuning of MOFs from preorganized
 heterometallic molecular complexes.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3676
_journal_page_last               3686
_journal_paper_doi               10.1039/c8dt05136d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C39 H42 Co Li N3 O9'
_chemical_formula_weight         762.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-12-05 deposited with the CCDC.    2019-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.248(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2469(4)
_cell_length_b                   29.1732(9)
_cell_length_c                   12.3612(4)
_cell_measurement_reflns_used    3908
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.27
_cell_measurement_theta_min      4.09
_cell_volume                     4052.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2017 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2017 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.845
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10599
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.498
_diffrn_reflns_theta_min         3.583
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         4784
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1681P)²+7.4099P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2430
_refine_ls_wR_factor_ref         0.2578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3780
_reflns_number_total             4784
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c8dt05136d2.cif
_cod_data_source_block           qch3cnco_sq
_cod_depositor_comments
'Adding full bibliography for 7049032--7049036.cif.'
_cod_database_code               7049035
_shelx_shelxl_version_number     2017/1
_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   0.839
_shelx_estimated_absorpt_t_max   0.949
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -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
_atom_site_refinement_flags_occupancy
Co1 Co 0.34678(7) 0.62460(2) 0.41358(6) 0.0265(3) Uani 0.5 1 d . . P
Li1 Li 0.34678(7) 0.62460(2) 0.41358(6) 0.0265(3) Uani 0.5 1 d . . P
O1 O 0.4117(2) 0.58300(9) 0.51884(18) 0.0442(6) Uani 1 1 d . . .
O2 O 0.29763(19) 0.60020(7) 0.65688(18) 0.0351(5) Uani 1 1 d . . .
O3 O 0.6805(2) 0.18801(8) 1.0627(2) 0.0433(6) Uani 1 1 d . . .
C1 C 0.3854(3) 0.58112(9) 0.6170(2) 0.0275(6) Uani 1 1 d . . .
C2 C 0.4670(2) 0.55452(9) 0.6925(2) 0.0232(5) Uani 1 1 d . . .
C3 C 0.5429(3) 0.52090(10) 0.6554(2) 0.0306(7) Uani 1 1 d . . .
H3 H 0.547237 0.515505 0.579847 0.037 Uiso 1 1 calc R U .
C4 C 0.6127(3) 0.49506(10) 0.7284(2) 0.0287(6) Uani 1 1 d . . .
H4 H 0.662179 0.471377 0.702708 0.034 Uiso 1 1 calc R U .
C5 C 0.6099(2) 0.50387(8) 0.8390(2) 0.0206(5) Uani 1 1 d . . .
C6 C 0.5362(2) 0.53856(9) 0.8753(2) 0.0241(6) Uani 1 1 d . . .
H6 H 0.535276 0.545323 0.950487 0.029 Uiso 1 1 calc R U .
C7 C 0.4642(2) 0.56333(9) 0.8027(2) 0.0245(6) Uani 1 1 d . . .
H7 H 0.412873 0.586383 0.828544 0.029 Uiso 1 1 calc R U .
C8 C 0.750000 0.50106(12) 1.000000 0.0212(7) Uani 1 2 d S T P
H8 H 0.750000 0.533624 0.999999 0.025 Uiso 1 2 calc R U P
C9 C 0.6843(2) 0.47765(8) 0.9194(2) 0.0205(5) Uani 1 1 d . . .
C10 C 0.6875(2) 0.42988(8) 0.9183(2) 0.0202(5) Uani 1 1 d . . .
H10 H 0.646801 0.413539 0.861609 0.024 Uiso 1 1 calc R U .
C11 C 0.750000 0.40594(11) 1.000000 0.0188(7) Uani 1 2 d S T P
C12 C 0.750000 0.35517(12) 1.000000 0.0199(7) Uani 1 2 d S T P
C13 C 0.7664(3) 0.33059(9) 0.9042(2) 0.0264(6) Uani 1 1 d . . .
H13 H 0.775325 0.346603 0.838110 0.032 Uiso 1 1 calc R U .
C14 C 0.7697(3) 0.28325(9) 0.9054(2) 0.0305(6) Uani 1 1 d . . .
H14 H 0.785582 0.267019 0.840904 0.037 Uiso 1 1 calc R U .
C15 C 0.750000 0.25915(13) 1.000000 0.0287(8) Uani 1 2 d S T P
C16 C 0.750000 0.20774(14) 1.000000 0.0345(10) Uani 1 2 d S T P
O1D O 0.4661(2) 0.62722(8) 0.29621(19) 0.0394(6) Uani 1 1 d . U .
N1D N 0.6255(4) 0.6325(2) 0.1944(4) 0.0848(10) Uani 1 1 d . U .
C1D C 0.5697(5) 0.6178(2) 0.2805(5) 0.0702(11) Uani 1 1 d . U .
C2D C 0.6379(5) 0.5863(2) 0.3577(5) 0.0787(11) Uani 1 1 d . U .
H2D1 H 0.719138 0.582422 0.333370 0.118 Uiso 1 1 calc R U .
H2D2 H 0.640411 0.599667 0.430467 0.118 Uiso 1 1 calc R U .
H2D3 H 0.598204 0.556421 0.359167 0.118 Uiso 1 1 calc R U .
C3D C 0.7487(5) 0.6226(2) 0.1699(6) 0.0886(12) Uani 1 1 d . U .
H3D1 H 0.767826 0.637458 0.101675 0.133 Uiso 1 1 calc R U .
H3D2 H 0.801723 0.634271 0.228402 0.133 Uiso 1 1 calc R U .
H3D3 H 0.759405 0.589375 0.163221 0.133 Uiso 1 1 calc R U .
C4D C 0.5623(5) 0.6619(3) 0.1153(5) 0.0873(12) Uani 1 1 d . U .
H4D1 H 0.615362 0.669662 0.056958 0.131 Uiso 1 1 calc R U .
H4D2 H 0.492372 0.645656 0.084941 0.131 Uiso 1 1 calc R U .
H4D3 H 0.536919 0.690049 0.150906 0.131 Uiso 1 1 calc R U .
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'
Li Li -0.0003 0.0001 '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'
Co Co 0.3494 0.9721 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O2 111.32(11) . 2_556 yes
O1 Co1 O1D 105.51(12) . . yes
O2 Co1 O1D 105.01(11) 2_556 . yes
O3 Co1 O1 125.11(11) 4_556 . yes
O3 Co1 O2 106.73(11) 4_556 2_556 yes
O3 Co1 O1D 100.98(11) 4_556 . yes
C1 O1 Co1 125.9(2) . . ?
C1 O2 Co1 130.03(19) . 2_556 ?
C16 O3 Co1 130.3(3) . 4_546 ?
O1 C1 C2 117.4(3) . . ?
O2 C1 O1 125.4(3) . . ?
O2 C1 C2 117.3(3) . . ?
C3 C2 C1 121.9(2) . . ?
C7 C2 C1 118.6(2) . . ?
C7 C2 C3 119.5(2) . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.3(2) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.2(3) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 119.1(2) . . ?
C4 C5 C9 121.9(2) . . ?
C6 C5 C9 119.0(2) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.6(2) . . ?
C7 C6 H6 119.7 . . ?
C2 C7 H7 119.9 . . ?
C6 C7 C2 120.2(2) . . ?
C6 C7 H7 119.9 . . ?
C9 C8 H8 119.3 . . ?
C9 C8 H8 119.3 2_657 . ?
C9 C8 C9 121.4(3) . 2_657 ?
C8 C9 C5 119.6(2) . . ?
C10 C9 C5 121.5(2) . . ?
C10 C9 C8 118.9(2) . . ?
C9 C10 H10 119.8 . . ?
C9 C10 C11 120.4(2) . . ?
C11 C10 H10 119.8 . . ?
C10 C11 C10 119.9(3) . 2_657 ?
C10 C11 C12 120.04(15) . . ?
C10 C11 C12 120.05(15) 2_657 . ?
C13 C12 C11 120.75(16) . . ?
C13 C12 C11 120.75(16) 2_657 . ?
C13 C12 C13 118.5(3) 2_657 . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.4(3) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 119.7 . . ?
C13 C14 C15 120.6(3) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 C14 119.2(4) . 2_657 ?
C14 C15 C16 120.38(18) 2_657 . ?
C14 C15 C16 120.39(18) . . ?
O3 C16 O3 125.7(4) 2_657 . ?
O3 C16 C15 117.2(2) . . ?
O3 C16 C15 117.2(2) 2_657 . ?
C1D O1D Co1 140.6(3) . . ?
C1D N1D C3D 125.9(6) . . ?
C1D N1D C4D 119.4(5) . . ?
C3D N1D C4D 114.7(5) . . ?
O1D C1D N1D 122.7(5) . . ?
O1D C1D C2D 120.0(5) . . ?
N1D C1D C2D 117.2(5) . . ?
C1D C2D H2D1 109.5 . . ?
C1D C2D H2D2 109.5 . . ?
C1D C2D H2D3 109.5 . . ?
H2D1 C2D H2D2 109.5 . . ?
H2D1 C2D H2D3 109.5 . . ?
H2D2 C2D H2D3 109.5 . . ?
N1D C3D H3D1 109.5 . . ?
N1D C3D H3D2 109.5 . . ?
N1D C3D H3D3 109.5 . . ?
H3D1 C3D H3D2 109.5 . . ?
H3D1 C3D H3D3 109.5 . . ?
H3D2 C3D H3D3 109.5 . . ?
N1D C4D H4D1 109.5 . . ?
N1D C4D H4D2 109.5 . . ?
N1D C4D H4D3 109.5 . . ?
H4D1 C4D H4D2 109.5 . . ?
H4D1 C4D H4D3 109.5 . . ?
H4D2 C4D H4D3 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 1.904(2) . yes
Co1 O2 1.947(2) 2_556 yes
Co1 O3 1.900(2) 4_556 yes
Co1 O1D 2.016(3) . yes
O1 C1 1.261(4) . ?
O2 C1 1.251(4) . ?
O3 C16 1.261(3) . ?
C1 C2 1.500(3) . ?
C2 C3 1.390(4) . ?
C2 C7 1.388(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.394(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.392(4) . ?
C5 C6 1.394(4) . ?
C5 C9 1.486(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.388(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.395(3) . ?
C8 C9 1.395(3) 2_657 ?
C9 C10 1.394(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.395(3) . ?
C11 C12 1.481(4) . ?
C12 C13 1.402(3) 2_657 ?
C12 C13 1.403(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.382(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.390(3) . ?
C15 C16 1.500(5) . ?
O1D C1D 1.219(6) . ?
N1D C1D 1.327(7) . ?
N1D C3D 1.459(8) . ?
N1D C4D 1.465(8) . ?
C1D C2D 1.512(8) . ?
C2D H2D1 0.9800 . ?
C2D H2D2 0.9800 . ?
C2D H2D3 0.9800 . ?
C3D H3D1 0.9800 . ?
C3D H3D2 0.9800 . ?
C3D H3D3 0.9800 . ?
C4D H4D1 0.9800 . ?
C4D H4D2 0.9800 . ?
C4D H4D3 0.9800 . ?
