Luminescent metal organic frameworks for sensing and gas adsorption studies
Verma, Pankaj; Singh, Udai P.; Butcher, Ray J.; CrystEngComm 21 (2019) 5470–; doi:10.1039/C9CE00732F

data_7233404
_publ_section_title
;
 Luminescent metal organic frameworks for sensing and gas adsorption
 studies
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              5470
_journal_paper_doi               10.1039/C9CE00732F
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety
'0.5(C180 H192 Cd8 N24 Na4 O60), 5(C3 H7 N O), 2(C2 H8 N)'
_chemical_formula_sum            'C109 H147 Cd4 N19 Na2 O35'
_chemical_formula_weight         2779.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2019-05-06 deposited with the CCDC.    2019-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.791(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.8360(14)
_cell_length_b                   24.094(2)
_cell_length_c                   17.7653(15)
_cell_measurement_temperature    296(2)
_cell_volume                     6375.2(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1076
_diffrn_reflns_av_unetI/netI     0.0912
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            70069
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.266
_diffrn_reflns_theta_min         0.845
_exptl_absorpt_coefficient_mu    0.747
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_F_000             2856
_refine_diff_density_max         2.269
_refine_diff_density_min         -1.417
_refine_diff_density_rms         0.401
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     804
_refine_ls_number_reflns         11620
_refine_ls_number_restraints     958
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0692
_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/[\s^2^(Fo^2^)+(0.1178P)^2^+8.2725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7171
_reflns_number_total             11620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00732f2.cif
_cod_data_source_block           ups2717(1)
_cod_depositor_comments
'Adding full bibliography for 7233404--7233405.cif.'
_cod_original_cell_volume        6375.3(9)
_cod_database_code               7233404
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.99951(17)
 0.00049(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid bond restraints
 O1S, N1S, C11S, C12S, C13S, O2S, N2S, C21S, C22S, C23S, O3S, N3S, C31S, C32S,
 C33S, O4S, N4S, C41S, C42S, C43S, O5S, N5S, C51S, C52S, C53S, O6S, N6S, C61S,
 C62S, C63S, N1E, C1E, C2E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1S \\sim N1S \\sim C11S \\sim C12S \\sim C13S \\sim O2S \\sim N2S \\sim C21S
\\sim C22S \\sim C23S \\sim O3S \\sim N3S \\sim C31S \\sim C32S \\sim C33S
\\sim O4S \\sim N4S \\sim C41S \\sim C42S \\sim C43S \\sim O5S \\sim N5S \\sim
C51S \\sim C52S \\sim C53S \\sim O6S \\sim N6S \\sim C61S \\sim C62S \\sim C63S
\\sim N1E \\sim C1E \\sim C2E: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O6S) \\sim Ueq, Uanis(N6S) \\sim Ueq, Uanis(C61S) \\sim Ueq, Uanis(C62S)
\\sim Ueq, Uanis(C63S) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{O1S, N1S, C11S, C12S, C13S} sigma for 1-2: 0.02, 1-3: 0.04
as
{O2S, N2S, C21S, C22S, C23S}
{O1S, N1S, C11S, C12S, C13S} sigma for 1-2: 0.02, 1-3: 0.04
as
{O3S, N3S, C31S, C32S, C33S}
{O1S, N1S, C11S, C12S, C13S} sigma for 1-2: 0.02, 1-3: 0.04
as
{O4S, N4S, C41S, C42S, C43S}
{O1S, N1S, C11S, C12S, C13S} sigma for 1-2: 0.02, 1-3: 0.04
as
{O5S, N5S, C51S, C52S, C53S}
{O1S, N1S, C11S, C12S, C13S} sigma for 1-2: 0.02, 1-3: 0.04
as
{O6S, N6S, C61S, C62S, C63S}
7. Others
 Fixed Sof: O6S(0.5) N6S(0.5) C61S(0.5) H61S(0.5) C62S(0.5) H62A(0.5)
 H62B(0.5) H62C(0.5) C63S(0.5) H63A(0.5) H63B(0.5) H63C(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C19(H19A,H19B), C28(H28A,H28B), N1E(H1EA,H1EB)
8.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), C12(H12), C14(H14), C16(H16), C21(H21), C23(H23),
 C25(H25), C30(H30), C32(H32), C34(H34), C11S(H11S), C21S(H21S), C31S(H31S),
 C41S(H41S), C51S(H51S), C61S(H61S)
8.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C12S(H12A,H12B,H12C),
 C13S(H13A,H13B,H13C), C22S(H22A,H22B,H22C), C23S(H23A,H23B,H23C), C32S(H32A,
 H32B,H32C), C33S(H33A,H33B,H33C), C42S(H42A,H42B,H42C), C43S(H43A,H43B,H43C),
 C52S(H52A,H52B,H52C), C53S(H53A,H53B,H53C), C62S(H62A,H62B,H62C), C63S(H63A,
 H63B,H63C), C1E(H1EC,H1ED,H1EE), C2E(H2EA,H2EB,H2EC)
;
_shelx_res_checksum              22276
_olex2_submission_special_instructions 'No special instructions were received'