#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:29:15 +0100 (dom 17 de nov de 2019) $
#$Revision: 230166 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/79/7057936.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_7057936
loop_
_publ_author_name
'Das, Debarati'
'Roy, Sandipan'
'Biradha, Kumar'
_publ_section_title
;
 Crystal engineering with isosteric triether and triamine linked aromatic
 tri-carboxylic acids: iso-structurality and synthon interplay in their
 co-crystals and salts with bis(pyridyl) derivatives
;
_journal_issue                   24
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19953
_journal_paper_doi               10.1039/C8NJ04600J
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C70 H70 N8 O16'
_chemical_formula_weight         1279.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/8
_audit_update_record
;
2018-09-10 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                103.912(18)
_cell_angle_beta                 97.77(2)
_cell_angle_gamma                100.062(19)
_cell_formula_units_Z            1
_cell_length_a                   6.874(5)
_cell_length_b                   12.860(9)
_cell_length_c                   18.821(12)
_cell_measurement_reflns_used    17207
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.994
_cell_measurement_theta_min      1.134
_cell_volume                     1562.6(19)
_computing_structure_refinement  'SHELXL-2014/8 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'BRUKER APEX-2 CCD'
_diffrn_measurement_method       hemisphere
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3298
_diffrn_reflns_av_unetI/netI     0.4563
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17207
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         1.134
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            needle
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       brown
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.38(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/8 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.825
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.825
_refine_ls_R_factor_all          0.2964
_refine_ls_R_factor_gt           0.1175
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2332
_refine_ls_wR_factor_ref         0.2829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1474
_reflns_number_total             5366
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8nj04600j2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7057935--7057944.cif.'
_cod_original_cell_volume        1562.6(18)
_cod_database_code               7057936
_shelx_shelxl_version_number     2014/8
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
O1M O 0.2027(10) 0.8434(5) 0.6338(4) 0.068(2) Uiso 1 1 d . .
H1M H 0.2985 0.8593 0.6139 0.102 Uiso 1 1 calc R U
C1M C 0.1623(15) 0.9440(7) 0.6801(6) 0.077(3) Uani 1 1 d . .
H1MA H 0.1249 0.9306 0.7250 0.115 Uiso 1 1 calc R U
H1MB H 0.0546 0.9656 0.6531 0.115 Uiso 1 1 calc R U
H1MC H 0.2810 1.0015 0.6926 0.115 Uiso 1 1 calc R U
O2M O 0.7030(10) 1.0562(5) 0.7265(3) 0.0591(19) Uani 1 1 d . .
H2M H 0.6580 1.0193 0.6835 0.089 Uiso 1 1 calc R U
C2M C 0.7010(14) 0.9843(8) 0.7760(5) 0.065(3) Uani 1 1 d . .
H2MA H 0.8274 0.9623 0.7817 0.098 Uiso 1 1 calc R U
H2MB H 0.5945 0.9205 0.7550 0.098 Uiso 1 1 calc R U
H2MC H 0.6799 1.0228 0.8238 0.098 Uiso 1 1 calc R U
C1A C 0.9031(13) 0.6464(8) 0.0752(6) 0.051(3) Uani 1 1 d . .
C2A C 0.9500(13) 0.7285(8) 0.1423(5) 0.053(3) Uani 1 1 d . .
H2A H 1.0425 0.7933 0.1479 0.064 Uiso 1 1 calc R U
C3A C 0.8548(14) 0.7115(8) 0.2014(5) 0.049(3) Uani 1 1 d . .
C4A C 0.7216(13) 0.6131(7) 0.1926(5) 0.051(3) Uani 1 1 d . .
H4A H 0.6727 0.5976 0.2334 0.062 Uiso 1 1 calc R U
C5A C 0.6613(13) 0.5381(8) 0.1236(6) 0.049(3) Uani 1 1 d . .
C6A C 0.7554(13) 0.5512(7) 0.0639(5) 0.049(3) Uani 1 1 d . .
H6A H 0.7208 0.4983 0.0182 0.059 Uiso 1 1 calc R U
O11A O 1.8786(9) 0.9485(5) 0.0666(4) 0.0592(19) Uani 1 1 d . .
H11A H 1.9822 0.9821 0.0584 0.089 Uiso 1 1 calc R U
O12A O 1.7770(8) 0.9413(5) -0.0528(4) 0.0527(18) Uani 1 1 d . .
N11A N 0.9845(12) 0.6662(6) 0.0138(5) 0.062(2) Uani 1 1 d . .
H11N H 0.9100 0.6348 -0.0293 0.075 Uiso 1 1 calc R U
C11A C 1.1724(14) 0.7311(7) 0.0137(5) 0.046(2) Uani 1 1 d . .
C12A C 1.3335(14) 0.7581(8) 0.0768(6) 0.060(3) Uani 1 1 d . .
H12A H 1.3146 0.7364 0.1195 0.072 Uiso 1 1 calc R U
C13A C 1.5189(15) 0.8178(7) 0.0720(5) 0.055(3) Uani 1 1 d . .
H13A H 1.6256 0.8327 0.1116 0.066 Uiso 1 1 calc R U
C14A C 1.5506(14) 0.8553(7) 0.0120(5) 0.049(3) Uani 1 1 d . .
C15A C 1.3830(15) 0.8300(7) -0.0499(6) 0.054(3) Uani 1 1 d . .
H15A H 1.3990 0.8547 -0.0918 0.065 Uiso 1 1 calc R U
C16A C 1.2053(16) 0.7708(7) -0.0463(5) 0.053(3) Uani 1 1 d . .
H16A H 1.0994 0.7560 -0.0862 0.063 Uiso 1 1 calc R U
C17A C 1.7368(14) 0.9149(7) 0.0037(6) 0.044(2) Uani 1 1 d . .
O21A O 0.3545(10) 0.8287(5) 0.5139(3) 0.0567(18) Uani 1 1 d . .
H21A H 0.3209 0.8340 0.5546 0.085 Uiso 1 1 calc R U
O22A O 0.6507(10) 0.9138(5) 0.5874(4) 0.062(2) Uani 1 1 d . .
N21A N 0.9254(11) 0.7890(6) 0.2702(4) 0.048(2) Uani 1 1 d . .
H21B H 1.0398 0.8326 0.2757 0.058 Uiso 1 1 calc R U
C21A C 0.8261(14) 0.8025(7) 0.3321(6) 0.050(3) Uani 1 1 d . .
C22A C 0.9431(15) 0.8464(7) 0.4028(6) 0.054(3) Uani 1 1 d . .
H22A H 1.0826 0.8611 0.4089 0.064 Uiso 1 1 calc R U
C23A C 0.8494(14) 0.8685(7) 0.4650(6) 0.047(2) Uani 1 1 d . .
H23A H 0.9298 0.9008 0.5118 0.056 Uiso 1 1 calc R U
C24A C 0.6451(15) 0.8447(7) 0.4598(6) 0.046(2) Uani 1 1 d . .
C25A C 0.5215(14) 0.8006(7) 0.3856(5) 0.048(3) Uani 1 1 d . .
H25A H 0.3822 0.7871 0.3802 0.058 Uiso 1 1 calc R U
C26A C 0.6104(14) 0.7784(6) 0.3223(6) 0.050(3) Uani 1 1 d . .
H26A H 0.5315 0.7488 0.2751 0.060 Uiso 1 1 calc R U
C27A C 0.5529(14) 0.8650(7) 0.5236(6) 0.045(3) Uani 1 1 d . .
O32A O -0.1928(9) 0.2777(6) 0.2740(4) 0.062(2) Uani 1 1 d . .
O31A O -0.1690(10) 0.4583(5) 0.3056(4) 0.0572(19) Uani 1 1 d . .
H31A H -0.2451 0.4426 0.3332 0.086 Uiso 1 1 calc R U
N31A N 0.5271(11) 0.4348(6) 0.1156(4) 0.051(2) Uani 1 1 d . .
H31B H 0.5422 0.3783 0.0833 0.062 Uiso 1 1 calc R U
C31A C 0.3764(14) 0.4198(8) 0.1559(5) 0.044(2) Uani 1 1 d . .
C32A C 0.3114(14) 0.3228(8) 0.1710(5) 0.050(3) Uani 1 1 d . .
H32A H 0.3733 0.2649 0.1549 0.060 Uiso 1 1 calc R U
C33A C 0.1572(14) 0.3078(8) 0.2092(5) 0.052(3) Uani 1 1 d . .
H33A H 0.1190 0.2402 0.2188 0.062 Uiso 1 1 calc R U
C34A C 0.0570(13) 0.3894(8) 0.2340(5) 0.043(2) Uani 1 1 d . .
C35A C 0.1234(14) 0.4907(8) 0.2207(5) 0.061(3) Uani 1 1 d . .
H35A H 0.0648 0.5491 0.2392 0.073 Uiso 1 1 calc R U
C36A C 0.2772(15) 0.5054(9) 0.1799(5) 0.058(3) Uani 1 1 d . .
H36A H 0.3139 0.5718 0.1686 0.070 Uiso 1 1 calc R U
C37A C -0.1108(14) 0.3708(8) 0.2725(5) 0.048(3) Uani 1 1 d . .
N11B N 0.5262(11) 0.4300(6) 0.3685(4) 0.047(2) Uani 1 1 d . .
C11B C 0.4100(14) 0.3432(8) 0.3815(5) 0.053(3) Uani 1 1 d . .
H11B H 0.4405 0.2752 0.3632 0.064 Uiso 1 1 calc R U
C12B C 0.2563(13) 0.3443(7) 0.4175(5) 0.045(2) Uani 1 1 d . .
H12B H 0.1880 0.2792 0.4241 0.054 Uiso 1 1 calc R U
C13B C 0.1959(13) 0.4432(7) 0.4458(5) 0.043(2) Uani 1 1 d . .
C14B C 0.3087(14) 0.5339(8) 0.4329(5) 0.052(3) Uani 1 1 d . .
H14B H 0.2783 0.6022 0.4501 0.062 Uiso 1 1 calc R U
C15B C 0.4675(13) 0.5257(8) 0.3947(5) 0.046(3) Uani 1 1 d . .
H15B H 0.5376 0.5891 0.3865 0.056 Uiso 1 1 calc R U
C16B C 0.0266(13) 0.4450(6) 0.4868(5) 0.047(2) Uani 1 1 d . .
H16B H 0.0589 0.4178 0.5298 0.056 Uiso 1 1 calc R U
H16C H -0.0916 0.3943 0.4548 0.056 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'
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'
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_3
C2A C1A C6A 121.7(9) .
C2A C1A N11A 119.2(9) .
C6A C1A N11A 118.4(9) .
C1A C2A C3A 118.7(9) .
C4A C3A N21A 122.8(9) .
C4A C3A C2A 119.6(9) .
N21A C3A C2A 116.7(9) .
C5A C4A C3A 120.4(9) .
C4A C5A C6A 121.0(9) .
C4A C5A N31A 119.8(9) .
C6A C5A N31A 118.2(9) .
C1A C6A C5A 117.7(9) .
C1A N11A C11A 128.3(9) .
C16A C11A N11A 120.9(9) .
C16A C11A C12A 118.5(9) .
N11A C11A C12A 120.6(9) .
C13A C12A C11A 118.0(9) .
C14A C13A C12A 122.9(9) .
C13A C14A C17A 125.2(9) .
C13A C14A C15A 117.9(9) .
C17A C14A C15A 116.9(9) .
C16A C15A C14A 119.6(9) .
C15A C16A C11A 123.1(10) .
O12A C17A O11A 118.9(9) .
O12A C17A C14A 127.1(9) .
O11A C17A C14A 113.9(8) .
C3A N21A C21A 126.0(8) .
C22A C21A N21A 118.0(9) .
C22A C21A C26A 120.4(10) .
N21A C21A C26A 121.4(9) .
C21A C22A C23A 119.6(9) .
C24A C23A C22A 122.9(9) .
C23A C24A C27A 122.2(10) .
C23A C24A C25A 117.7(9) .
C27A C24A C25A 120.1(9) .
C26A C25A C24A 120.7(9) .
C25A C26A C21A 118.6(9) .
O22A C27A O21A 119.6(9) .
O22A C27A C24A 122.6(9) .
O21A C27A C24A 117.8(10) .
C31A N31A C5A 124.9(8) .
C32A C31A N31A 122.4(9) .
C32A C31A C36A 117.7(9) .
N31A C31A C36A 119.9(9) .
C31A C32A C33A 121.9(9) .
C32A C33A C34A 122.2(9) .
C33A C34A C35A 117.1(9) .
C33A C34A C37A 121.4(9) .
C35A C34A C37A 121.5(9) .
C34A C35A C36A 120.8(10) .
C35A C36A C31A 120.2(10) .
O32A C37A O31A 121.9(9) .
O32A C37A C34A 122.2(9) .
O31A C37A C34A 115.8(9) .
C11B N11B C15B 112.9(8) .
C12B C11B N11B 127.0(9) .
C11B C12B C13B 120.7(8) .
C14B C13B C12B 114.3(9) .
C14B C13B C16B 124.8(8) .
C12B C13B C16B 120.9(8) .
C13B C14B C15B 121.4(9) .
N11B C15B C14B 123.7(9) .
C13B C16B C16B 116.1(9) 2_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1M C1M 1.470(10) .
O2M C2M 1.461(10) .
C1A C2A 1.395(12) .
C1A C6A 1.399(11) .
C1A N11A 1.409(11) .
C2A C3A 1.405(12) .
C3A C4A 1.386(11) .
C3A N21A 1.396(10) .
C4A C5A 1.378(12) .
C5A C6A 1.400(12) .
C5A N31A 1.441(10) .
O11A C17A 1.353(10) .
O12A C17A 1.243(9) .
N11A C11A 1.410(11) .
C11A C16A 1.376(11) .
C11A C12A 1.439(12) .
C12A C13A 1.394(12) .
C13A C14A 1.359(11) .
C14A C17A 1.421(12) .
C14A C15A 1.455(12) .
C15A C16A 1.341(11) .
O21A C27A 1.335(10) .
O22A C27A 1.249(11) .
N21A C21A 1.417(11) .
C21A C22A 1.388(12) .
C21A C26A 1.438(12) .
C22A C23A 1.405(12) .
C23A C24A 1.369(12) .
C24A C27A 1.423(12) .
C24A C25A 1.457(12) .
C25A C26A 1.403(11) .
O32A C37A 1.239(10) .
O31A C37A 1.305(10) .
N31A C31A 1.378(10) .
C31A C32A 1.359(11) .
C31A C36A 1.409(12) .
C32A C33A 1.371(11) .
C33A C34A 1.378(12) .
C34A C35A 1.394(12) .
C34A C37A 1.458(12) .
C35A C36A 1.402(12) .
N11B C11B 1.347(11) .
N11B C15B 1.362(11) .
C11B C12B 1.331(11) .
C12B C13B 1.411(11) .
C13B C14B 1.376(11) .
C13B C16B 1.481(11) .
C14B C15B 1.392(11) .
C16B C16B 1.508(15) 2_566
