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_7219965
_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_moiety
'C48 H53 N5 O32 S4 Sm2, C20 H20 N6 O12 Sm, C10 H8 N2 O2, 12(H2 O), N O3'
_chemical_formula_sum            'C78 H105 N14 O61 S4 Sm3'
_chemical_formula_weight         2793.95
_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             2015-03-11
_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                116.848(2)
_cell_angle_beta                 91.344(2)
_cell_angle_gamma                90.928(2)
_cell_formula_units_Z            2
_cell_length_a                   15.9282(12)
_cell_length_b                   18.6918(15)
_cell_length_c                   19.2219(15)
_cell_measurement_reflns_used    9603
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      2.18
_cell_volume                     5102.3(7)
_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      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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     0.0376
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            39868
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.188
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.903
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_description       block
_exptl_crystal_F_000             2794
_exptl_crystal_recrystallization_method
'Crsytal were obtained from evaporating the solution at room temperature'
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.220
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1522
_refine_ls_number_reflns         39868
_refine_ls_number_restraints     1338
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+16.6018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                36891
_reflns_number_total             39868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00153f2.cif
_cod_data_source_block           smcalix
_cod_depositor_comments
'Adding full bibliography for 7219964--7219965.cif.'
_cod_database_code               7219965
_shelx_estimated_absorpt_t_max   0.702
_shelx_estimated_absorpt_t_min   0.421
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.654(2) 0.1989(16) 0.1467(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H,H,H,H,H,H,H) groups
3. Restrained distances
 N14-O49A
 1.23 with sigma of 0.01
 N14-O49B
 1.23 with sigma of 0.01
 H5B-O5 = H5A-O5
 0.83 with sigma of 0.01
 O6-H6A = O6-H6B
 0.83 with sigma of 0.01
 H14A-O14 = H14B-O14
 0.83 with sigma of 0.01
 H15A-O15 = H15B-O15
 0.83 with sigma of 0.01
 H16B-O16 = H16A-O16
 0.83 with sigma of 0.01
 H17A-O17 = H17B-O17
 0.83 with sigma of 0.01
 H18A-O18 = H18B-O18
 0.83 with sigma of 0.01
 H40B-O40 = H40A-O40
 0.83 with sigma of 0.01
 H41A-O41 = H41B-O41
 0.83 with sigma of 0.01
 H42A-O42 = H42B-O42
 0.83 with sigma of 0.01
 H43B-O43 = H43A-O43
 0.83 with sigma of 0.01
 H50B-O50 = H50A-O50
 0.83 with sigma of 0.01
 H51A-O51 = H51B-O51
 0.83 with sigma of 0.01
 H53B-O53 = H53A-O53
 0.83 with sigma of 0.01
 H54B-O54 = H54A-O54
 0.83 with sigma of 0.01
 H56A-O56 = H56B-O56
 0.83 with sigma of 0.01
 H57D-O57 = H57C-O57
 0.83 with sigma of 0.01
 H5A-H5B
 1.35 with sigma of 0.02
 H6A-H6B
 1.35 with sigma of 0.02
 H14A-H14B
 1.35 with sigma of 0.02
 H15A-H15B
 1.35 with sigma of 0.02
 H16B-H16A
 1.35 with sigma of 0.02
 H17A-H17B
 1.35 with sigma of 0.02
 H18A-H18B
 1.35 with sigma of 0.02
 H40B-H40A
 1.35 with sigma of 0.02
 H41B-H41A
 1.35 with sigma of 0.02
 H42A-H42B
 1.35 with sigma of 0.02
 H43A-H43B
 1.35 with sigma of 0.02
 H50A-H50B
 1.35 with sigma of 0.02
 H51A-H51B
 1.35 with sigma of 0.02
 H53B-H53A
 1.35 with sigma of 0.02
 H54B-H54A
 1.35 with sigma of 0.02
 H56A-H56B
 1.35 with sigma of 0.02
 H57D-H57C
 1.35 with sigma of 0.02
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(O55B)=Sof(O49B)=Sof(O58B)=Sof(O61B)=1-FVAR(1)
 Sof(O55A)=Sof(O49A)=Sof(O61A)=Sof(O58A)=FVAR(1)
7.a Free rotating group:
 O54(H54A,H54B), O50(H50A,H50B)
7.b Rotating group:
 O6(H6A,H6B), O43(H43A,H43B), O40(H40A,H40B), O15(H15A,H15B), O41(H41A,H41B),
 O17(H17A,H17B), O5(H5A,H5B), O14(H14A), O16(H16A,H16B), O18(H18A,H18B),
 O42(H42A,H42B)
7.c Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C57(H57A,H57B), C64(H64A,H64B), C78(H78A,H78B)
7.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C51(H51), C66(H66), C29(H29), C73(H73), C16(H16), C47(H47), C32(H32A),
  C26(H26), C19(H19), C15(H15), C53(H53), C24(H24), C37(H37), C7(H7), C59(H59),
 C10(H10), C5(H5), C14(H14), C22(H22), C30(H30), C41(H41), C31(H31), C4(H4),
 C25(H25), C50(H50), C35(H35A), C44(H44), C20(H20), C49(H49), C17(H17), C6(H6),
 C42(H42), C61(H61), C12(H12), C34(H34A), C27(H27), C36(H36), C1(H1), C11(H11),
 C68(H68), C21(H21), C2(H2), C45(H45), C75(H75), C46(H46), C40(H40), C39(H39)
7.e Idealised tetrahedral OH refined as rotating group:
 O35(H35), O32(H32), O34(H34)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'