Template effect of innocent and coordinating anions on the formation of interpenetrated 2D and 3D networks: methyl orange and iodine sorption studies
Baig, Fayaz; Rangan, Krishnan; Eappen, Shibu M.; Mandal, Sanjay K.; Sarkar, Madhushree; CrystEngComm 22 (2020) 751–766; doi:10.1039/C9CE00998A

data_7239710
_publ_section_title
;
 Template effect of innocent and coordinating anions on the formation of
 interpenetrated 2D and 3D networks: methyl orange and iodine sorption
 studies
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              751
_journal_page_last               766
_journal_paper_doi               10.1039/C9CE00998A
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'C56 H64 Cd2 N16 O4, 4(Cl O4), 5(H2 O)'
_chemical_formula_sum            'C56 H74 Cd2 Cl4 N16 O25'
_chemical_formula_weight         1737.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-06 deposited with the CCDC.	2019-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                71.776(3)
_cell_angle_beta                 87.979(3)
_cell_angle_gamma                85.994(4)
_cell_formula_units_Z            2
_cell_length_a                   11.4937(6)
_cell_length_b                   14.6527(7)
_cell_length_c                   22.6545(6)
_cell_measurement_reflns_used    11051
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.0790
_cell_measurement_theta_min      3.7910
_cell_volume                     3614.7(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.910
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19007
_diffrn_reflns_point_group_measured_fraction_full 0.910
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        59.996
_diffrn_reflns_theta_max         59.996
_diffrn_reflns_theta_min         3.856
_exptl_absorpt_coefficient_mu    6.828
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       block
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.677
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     970
_refine_ls_number_reflns         9778
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+16.6508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8586
_reflns_number_total             9778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00998a2.cif
_cod_data_source_block           cp1
_cod_depositor_comments
;Adding full bibliography for 7239708--7239712.cif.

 Adding full bibliography for 7239708--7239712.cif.
;
_cod_database_code               7239710
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O4-H4A = O4-H4B
 0.85 with sigma of 0.02
 O3-H3A = O3-H3B
 0.85 with sigma of 0.02
 O1-H1A = O1-H1B
 0.85 with sigma of 0.02
 O2-H2A = O2-H2B
 0.85 with sigma of 0.02
 H4A-H4B
 1.34 with sigma of 0.04
 H3A-H3B
 1.34 with sigma of 0.04
 H1A-H1B
 1.34 with sigma of 0.04
 H2A-H2B
 1.34 with sigma of 0.04
 Cl4-O20 \\sim Cl4-O21
 with sigma of 0.02
 Cd2-H4A \\sim Cd2-H4B
 with sigma of 0.02
 Cd2-H3A \\sim Cd2-H3B
 with sigma of 0.02
 Cd1-H1A \\sim Cd1-H1B
 with sigma of 0.02
 Cd1-H2A \\sim Cd1-H2B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O26) \\sim Ueq: with sigma of 0.2 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 Cl4, O17, O18, O19, O20, O21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O21)=1-FVAR(1)
 Sof(O20)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C22(H22), C23(H23), C26(H26),
  C27(H27), C29(H29), C31(H31), C35(H35), C36(H36), C37(H37), C39(H39),
 C40(H40), C41(H41), C45(H45), C47(H47), C49(H49), C50(H50), C52(H52), C53(H53),
  C54(H54)
6.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C55(H55A,H55B,H55C), C56(H56A,
 H56B,H56C)
;
_shelx_res_checksum              97720
_olex2_submission_special_instructions 'No special instructions were received'