#------------------------------------------------------------------------------
#$Date: 2020-09-06 12:44:35 +0300 (Sun, 06 Sep 2020) $
#$Revision: 256110 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705125.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_7705125
loop_
_publ_author_name
'Houlihan, Joanna C. C.'
'Moratti, Stephen C.'
'Hanton, Lyall R.'
_publ_section_title
;
 Formation of a robust, double-walled LiMOF from an L-shaped
 di-substituted N-heterocyclic adamantane-based ligand.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12009
_journal_page_last               12017
_journal_paper_doi               10.1039/d0dt02437f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C24 H26.42 N2 O2.21'
_chemical_formula_weight         378.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-08-03 deposited with the CCDC.	2020-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2609(4)
_cell_length_b                   6.7138(3)
_cell_length_c                   25.8248(8)
_cell_measurement_reflns_used    3692
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      72.1110
_cell_measurement_theta_min      4.2540
_cell_volume                     1952.44(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector_area_resol_mean 5.1725
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            9991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.470
_diffrn_reflns_theta_min         4.283
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       rhomboid
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         1954
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0416
_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)+(0.0643P)²+0.5772P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1172
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1601
_reflns_number_total             1954
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02437f2.cif
_cod_data_source_block           Compound9
_cod_depositor_comments
'Adding full bibliography for 7705120--7705129.cif.'
_cod_database_code               7705125
_shelx_shelxl_version_number     2018/3
_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.
;
_exptl_absorpt_special_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3776(2) 0.750000 0.25457(8) 0.0316(5) Uani 1 2 d S T P . .
C2 C 0.35228(19) 0.750000 0.31150(7) 0.0232(5) Uani 1 2 d S T P . .
C3 C 0.44593(18) 0.750000 0.34672(8) 0.0216(4) Uani 1 2 d S T P . .
H3 H 0.524018 0.750000 0.335002 0.026 Uiso 1 2 calc R U P . .
C4 C 0.42205(17) 0.750000 0.39913(7) 0.0186(4) Uani 1 2 d S T P . .
H4 H 0.483960 0.750000 0.422968 0.022 Uiso 1 2 calc R U P . .
C5 C 0.23785(18) 0.750000 0.33154(8) 0.0233(5) Uani 1 2 d S T P . .
H5 H 0.174682 0.750000 0.308340 0.028 Uiso 1 2 calc R U P . .
C6 C 0.30420(17) 0.750000 0.41618(7) 0.0176(4) Uani 1 2 d S T P . .
C7 C 0.26958(16) 0.750000 0.47314(7) 0.0161(4) Uani 1 2 d S T P . .
C8 C 0.37849(16) 0.750000 0.50914(7) 0.0158(4) Uani 1 2 d S T P . .
H8A H 0.426505 0.866881 0.502132 0.019 Uiso 0.5 1 calc R U P . .
H8B H 0.426505 0.633119 0.502132 0.019 Uiso 0.5 1 calc R U P . .
C9 C 0.26435(12) 0.5631(2) 0.57716(5) 0.0192(3) Uani 1 1 d . . . . .
H9A H 0.310896 0.443960 0.570829 0.023 Uiso 1 1 calc R U . . .
H9B H 0.239486 0.562075 0.613125 0.023 Uiso 1 1 calc R U . . .
C10 C 0.15455(12) 0.5637(2) 0.54180(5) 0.0207(3) Uani 1 1 d . . . . .
H10 H 0.106670 0.444698 0.548711 0.025 Uiso 1 1 calc R U . . .
C11 C 0.08026(17) 0.750000 0.55258(8) 0.0230(5) Uani 1 2 d S T P . .
H11A H 0.054379 0.750002 0.588410 0.028 Uiso 1 2 calc R U P . .
H11B H 0.010306 0.750000 0.530667 0.028 Uiso 1 2 calc R U P . .
C12 C 0.19460(12) 0.5627(2) 0.48502(5) 0.0196(3) Uani 1 1 d . . . . .
H12A H 0.125541 0.559859 0.462583 0.023 Uiso 1 1 calc R U . . .
H12B H 0.241336 0.444162 0.478245 0.023 Uiso 1 1 calc R U . . .
C13 C 0.34113(16) 0.750000 0.56653(7) 0.0163(4) Uani 1 2 d S T P . .
C14 C 0.44887(17) 0.750000 0.60195(7) 0.0171(4) Uani 1 2 d S T P . .
C15 C 0.43409(18) 0.750000 0.65612(7) 0.0215(4) Uani 1 2 d S T P . .
H15 H 0.358350 0.750000 0.670471 0.026 Uiso 1 2 calc R U P . .
C16 C 0.5326(2) 0.750000 0.68758(7) 0.0240(5) Uani 1 2 d S T P . .
H16 H 0.523977 0.750000 0.723396 0.029 Uiso 1 2 calc R U P . .
C17 C 0.65132(17) 0.750000 0.61150(7) 0.0177(4) Uani 1 2 d S T P . .
H17 H 0.726139 0.750000 0.596257 0.021 Uiso 1 2 calc R U P . .
C18 C 0.64557(18) 0.750000 0.66534(7) 0.0200(4) Uani 1 2 d S T P . .
C19 C 0.75424(19) 0.750000 0.69825(8) 0.0250(5) Uani 1 2 d S T P . .
C20 C 0.8741(2) 0.750000 0.67258(9) 0.0352(6) Uani 1 2 d S T P . .
H20B H 0.883045 0.630838 0.652377 0.050 Uiso 1 1 d . U . . .
H20C H 0.935069 0.750000 0.698516 0.050 Uiso 1 2 d S U P . .
C21 C 0.2760(2) 0.750000 0.21695(8) 0.0359(6) Uani 1 2 d S T P . .
H21A H 0.306362 0.750000 0.182211 0.054 Uiso 1 2 calc R U P . .
H21B H 0.228317 0.866750 0.222281 0.054 Uiso 0.5 1 calc R U P . .
H21C H 0.228317 0.633250 0.222280 0.054 Uiso 0.5 1 calc R U P . .
N1 N 0.55671(14) 0.750000 0.58015(6) 0.0174(4) Uani 1 2 d S T P . .
N2 N 0.21287(15) 0.750000 0.38234(6) 0.0223(4) Uani 1 2 d S T P . .
O1 O 0.74470(15) 0.750000 0.74550(6) 0.0350(4) Uani 1 2 d S T P . .
O2 O 0.47931(17) 0.750000 0.23965(6) 0.0587(6) Uani 1 2 d S T P . .
O3 O 0.0318(7) 0.250000 0.6275(3) 0.052(4) Uani 0.211(6) 2 d DS T P . .
H3A H 0.027(17) 0.250000 0.6593(7) 0.078 Uiso 0.211(6) 2 d DS U P . .
H3B H -0.039(4) 0.250000 0.620(7) 0.078 Uiso 0.211(6) 2 d DS U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O2 C1 C2 119.6(2) . . ?
O2 C1 C21 121.1(2) . . ?
C2 C1 C21 119.4(2) . . ?
C5 C2 C3 117.33(18) . . ?
C5 C2 C1 122.85(19) . . ?
C3 C2 C1 119.81(19) . . ?
C4 C3 C2 119.55(19) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C6 119.59(18) . . ?
C3 C4 H4 120.2 . . ?
C6 C4 H4 120.2 . . ?
N2 C5 C2 123.98(18) . . ?
N2 C5 H5 118.0 . . ?
C2 C5 H5 118.0 . . ?
N2 C6 C4 121.29(18) . . ?
N2 C6 C7 115.52(17) . . ?
C4 C6 C7 123.20(17) . . ?
C6 C7 C8 112.32(15) . . ?
C6 C7 C12 109.39(10) . 7_575 ?
C8 C7 C12 108.38(10) . 7_575 ?
C6 C7 C12 109.38(10) . . ?
C8 C7 C12 108.39(10) . . ?
C12 C7 C12 108.92(15) 7_575 . ?
C7 C8 C13 111.32(15) . . ?
C7 C8 H8A 109.4 . . ?
C13 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
C13 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C10 C9 C13 109.98(12) . . ?
C10 C9 H9A 109.7 . . ?
C13 C9 H9A 109.7 . . ?
C10 C9 H9B 109.7 . . ?
C13 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
C11 C10 C12 109.75(12) . . ?
C11 C10 C9 109.49(12) . . ?
C12 C10 C9 109.35(11) . . ?
C11 C10 H10 109.4 . . ?
C12 C10 H10 109.4 . . ?
C9 C10 H10 109.4 . . ?
C10 C11 C10 109.65(15) . 7_575 ?
C10 C11 H11A 109.7 . . ?
C10 C11 H11A 109.7 7_575 . ?
C10 C11 H11B 109.7 . . ?
C10 C11 H11B 109.7 7_575 . ?
H11A C11 H11B 108.2 . . ?
C10 C12 C7 110.30(11) . . ?
C10 C12 H12A 109.6 . . ?
C7 C12 H12A 109.6 . . ?
C10 C12 H12B 109.6 . . ?
C7 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
C14 C13 C8 111.17(15) . . ?
C14 C13 C9 109.81(10) . 7_575 ?
C8 C13 C9 108.85(10) . 7_575 ?
C14 C13 C9 109.81(10) . . ?
C8 C13 C9 108.85(10) . . ?
C9 C13 C9 108.28(15) 7_575 . ?
N1 C14 C15 121.66(17) . . ?
N1 C14 C13 118.11(16) . . ?
C15 C14 C13 120.24(17) . . ?
C16 C15 C14 119.45(18) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C18 119.48(17) . . ?
C15 C16 H16 120.3 . . ?
C18 C16 H16 120.3 . . ?
N1 C17 C18 124.57(18) . . ?
N1 C17 H17 117.7 . . ?
C18 C17 H17 117.7 . . ?
C17 C18 C16 116.96(18) . . ?
C17 C18 C19 122.12(18) . . ?
C16 C18 C19 120.92(17) . . ?
O1 C19 C18 119.76(19) . . ?
O1 C19 C20 121.19(19) . . ?
C18 C19 C20 119.04(17) . . ?
C19 C20 H20B 109.50(15) . . ?
C19 C20 H20C 109.5(2) . . ?
H20B C20 H20C 107.70(15) . . ?
C19 C20 H20B 109.50(15) . 7_575 ?
H20B C20 H20B 112.8(2) . 7_575 ?
H20C C20 H20B 107.71(15) . 7_575 ?
C1 C21 H21A 109.5 . . ?
C1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C17 N1 C14 117.89(16) . . ?
C5 N2 C6 118.26(17) . . ?
H3A O3 H3B 101(10) . . ?
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
C1 O2 1.209(3) . ?
C1 C2 1.498(3) . ?
C1 C21 1.501(3) . ?
C2 C5 1.389(3) . ?
C2 C3 1.393(3) . ?
C3 C4 1.380(3) . ?
C3 H3 0.9300 . ?
C4 C6 1.398(3) . ?
C4 H4 0.9300 . ?
C5 N2 1.342(3) . ?
C5 H5 0.9300 . ?
C6 N2 1.350(2) . ?
C6 C7 1.522(2) . ?
C7 C8 1.539(2) . ?
C7 C12 1.5454(17) 7_575 ?
C7 C12 1.5454(17) . ?
C8 C13 1.541(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.5371(18) . ?
C9 C13 1.5486(17) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.5305(18) . ?
C10 C12 1.5342(17) . ?
C10 H10 0.9800 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.520(3) . ?
C14 N1 1.339(2) . ?
C14 C15 1.409(3) . ?
C15 C16 1.375(3) . ?
C15 H15 0.9300 . ?
C16 C18 1.396(3) . ?
C16 H16 0.9300 . ?
C17 N1 1.338(2) . ?
C17 C18 1.392(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.490(3) . ?
C19 O1 1.225(3) . ?
C19 C20 1.504(3) . ?
C20 H20B 0.9604(13) . ?
C20 H20C 0.959(2) . ?
C20 H20B 0.9604(13) 7_575 ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
O3 H3A 0.821(10) . ?
O3 H3B 0.821(11) . ?
