Novel mixed 1D‒2D lanthanide coordination polymers based on p-sulfonatocalix[4]arene and 4,4′-bipyridine-N,N′-dioxide where p-sulfonatocalix[4]arene acts as a guest
Husain, Ahmad; Oliver, Clive L.; CrystEngComm 17 (2015) 3023–; doi:10.1039/C5CE00153F

data_7219964
_publ_section_title
;
 Novel mixed 1D--2D lanthanide coordination polymers based on
 p-sulfonatocalix[4]arene and 4,4&#x2032;-bipyridine-N,N&#x2032;-dioxide
 where p-sulfonatocalix[4]arene acts as a guest
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              3023
_journal_paper_doi               10.1039/C5CE00153F
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C78 H105 N14 Nd3 O61 S4'
_chemical_formula_weight         2774.61
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-16 deposited with the CCDC.
2015-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                116.971(2)
_cell_angle_beta                 91.384(2)
_cell_angle_gamma                90.880(2)
_cell_formula_units_Z            2
_cell_length_a                   15.9870(15)
_cell_length_b                   18.7220(18)
_cell_length_c                   19.3040(19)
_cell_measurement_reflns_used    4920
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      2.51
_cell_volume                     5145.7(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25582
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.441
_diffrn_reflns_theta_min         1.184
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.688
_exptl_absorpt_correction_T_max  0.9553
_exptl_absorpt_correction_T_min  0.8498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0927 before and 0.0770 after correction.
The Ratio of minimum to maximum transmission is 0.8896.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_description       block
_exptl_crystal_F_000             2780
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.291
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1503
_refine_ls_number_reflns         25582
_refine_ls_number_restraints     1283
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0537P)^2^+2.2591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19785
_reflns_number_total             25582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00153f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7219964--7219965.cif.'
_cod_database_code               7219964
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.474
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5075(6) 0.4925(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H,H,H,H,H,H,H,H,H,H,H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Restrained distances
 O11-H11B = O11-H11A
 0.87 with sigma of 0.02
 O12-H12A = O12-H12B
 0.87 with sigma of 0.02
 O17-H17A = O17-H17B
 0.87 with sigma of 0.02
 O24-H24B = O24-H24A
 0.87 with sigma of 0.02
 O50-H50A = O50-H50B
 0.87 with sigma of 0.02
 O52-H52B = O52-H52A
 0.87 with sigma of 0.02
 O51-H51A = O51-H51B
 0.87 with sigma of 0.02
 H11B-H11A
 1.35 with sigma of 0.04
 H12A-H12B
 1.35 with sigma of 0.04
 H17A-H17B
 1.35 with sigma of 0.04
 H24B-H24A
 1.35 with sigma of 0.04
 H50A-H50B
 1.35 with sigma of 0.04
 H52B-H52A
 1.35 with sigma of 0.04
 H51A-H51B
 1.35 with sigma of 0.04
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
6. Others
 Sof(O57B)=1-FVAR(1)
 Sof(O57A)=FVAR(1)
 Sof(O58B)=1-FVAR(2)
 Sof(O58A)=FVAR(2)
 Sof(O59B)=1-FVAR(3)
 Sof(O59A)=FVAR(3)
 Sof(O60B)=1-FVAR(4)
 Sof(O60A)=FVAR(4)
 Sof(O61B)=1-FVAR(5)
 Sof(O61A)=FVAR(5)
7.a Free rotating group:
 O53(H53A,H53B), O54(H54), O55(H55A,H55B)
7.b Rotating group:
 O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B), O23(H23A,H23B), O25(H25A,
 H25B), O26(H26A,H26B), O27(H27A,H27B)
7.c Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C54(H54A,H54B), C61(H61A,H61B), C68(H68A,H68B)
7.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21),
  C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30),
 C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40),
  C41(H41A), C43(H43A), C49(H49), C51(H51), C56(H56), C58(H58), C63(H63),
 C65(H65), C69(H69), C70(H70), C72(H72), C73(H73), C74(H74), C75(H75), C77(H77),
  C78(H78)
7.e Idealised tetrahedral OH refined as rotating group:
 O41(H41), O43(H43), O44(H44)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id 2
_olex2_submission_special_instructions 'No special instructions were received'