Influence of lower rim C-methyl group on crystal forms and metal complexation of resorcinarene bis-crown-5
Helttunen, Kaisa; Tero, Tiia-Riikka; Nissinen, Maija; CrystEngComm 17 (2015) 3667–; doi:10.1039/C5CE00311C

data_7220275
_publ_section_title
;
 Influence of lower rim C-methyl group on crystal forms and metal
 complexation of resorcinarene bis-crown-5
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              3667
_journal_paper_doi               10.1039/C5CE00311C
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C52 H68 Cs2 F6 O14 P, F6 P, 0.5(C3 H6 O)'
_chemical_formula_sum            'C53.5 H71 Cs2 F12 O14.5 P2'
_chemical_formula_weight         1501.86
_chemical_name_common
'di-cesium C-methyl tetramethoxy resorcinarene bis-crown-5 bis(hexafluorophosphate) acetone solvate'
_chemical_name_systematic
'di-cesium C-methyl tetramethoxy resorcinarene bis-crown-5 bis(hexafluorophosphate) acetone solvate'
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2015-01-05 deposited with the CCDC.
2015-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                80.0591(19)
_cell_angle_beta                 89.3602(19)
_cell_angle_gamma                88.9220(18)
_cell_formula_units_Z            2
_cell_length_a                   13.2706(3)
_cell_length_b                   15.2318(3)
_cell_length_c                   16.1051(4)
_cell_measurement_reflns_used    9620
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      75.0980
_cell_measurement_theta_min      4.3420
_cell_volume                     3205.86(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
  1 omega  -49.00   33.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   37.0000  -60.0000 164

  2 omega  -94.00   -6.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513  125.0000   30.0000 176

  3 omega   44.00   81.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6513 -125.0000  -30.0000 74

  4 omega -124.00  -25.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -50.5000  -45.0000  150.0000 198

  5 omega -126.00  -87.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -50.5000 -111.0000 -150.0000 78

  6 omega   36.00  116.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000    0.0000 160

  7 omega   40.00   99.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -150.0000 118

  8 omega   48.00  109.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -120.0000 122

  9 omega   99.00  178.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000  -30.0000 158

 10 omega   82.00  109.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  120.0000 54

 11 omega   36.00   91.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  150.0000 110

 12 omega   37.00  116.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -150.0000 158

 13 omega   44.00   90.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -60.0000 92

 14 omega  113.00  161.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  -90.0000 96

 15 omega   29.00   59.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  120.0000 60

 16 omega   62.00  178.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   15.0000   90.0000 232

 17 omega   38.00  120.00   0.5000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000   30.0000 164
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0401926000
_diffrn_orient_matrix_UB_12      0.0688660000
_diffrn_orient_matrix_UB_13      -0.0737824000
_diffrn_orient_matrix_UB_21      0.0729126000
_diffrn_orient_matrix_UB_22      0.0345859000
_diffrn_orient_matrix_UB_23      0.0602902000
_diffrn_orient_matrix_UB_31      0.0809347000
_diffrn_orient_matrix_UB_32      -0.0678832000
_diffrn_orient_matrix_UB_33      -0.0187938000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21759
_diffrn_reflns_theta_full        75.99
_diffrn_reflns_theta_max         75.99
_diffrn_reflns_theta_min         4.36
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.169
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone/dichloromethane'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.737
_refine_diff_density_min         -1.665
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         12904
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+2.2451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                11350
_reflns_number_total             12904
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00311c2.cif
_cod_data_source_block           1-Cs2
_cod_depositor_comments
'Adding full bibliography for 7220270--7220279.cif.'
_cod_original_formula_sum        'C53.50 H71 Cs2 F12 O14.50 P2'
_cod_database_code               7220275
_chemical_oxdiff_formula         C52H68O14Cs2P2F6
_reflns_odcompleteness_completeness 99.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C83-C82
 2.5 with sigma of 0.04
 C82-O80
 2.3 with sigma of 0.04
 C83-O80
 2.3 with sigma of 0.04
3. Rigid bond restraints
 C57A, C57
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F1, F2, F3, F4, F5, F6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C57A \\sim C57: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
Uanis(C83) \\sim Ueq: with sigma of 0.5 and sigma for terminal atoms of 0.2
Uanis(O80) \\sim Ueq: with sigma of 0.5 and sigma for terminal atoms of 0.2
5. Others
 Sof(O56A)=Sof(H54C)=Sof(H54D)=Sof(C55A)=Sof(H55C)=Sof(H55D)=Sof(C57A)=
 Sof(H57C)=Sof(H57D)=Sof(H58C)=Sof(H58D)=1-FVAR(1)
 Sof(O56)=Sof(H54A)=Sof(H54B)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C57)=Sof(H57A)=
 Sof(H57B)=Sof(H58A)=Sof(H58B)=FVAR(1)
 Fixed Sof: O80(0.5) C81(0.5) C82(0.5) H82A(0.5) H82B(0.5) H82C(0.5) C83(0.5)
 H83A(0.5) H83B(0.5) H83C(0.5)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C21(H21), C28(H28)
6.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,
 H43B), C44(H44A,H44B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
 C49(H49A,H49B), C51(H51A,H51B), C52(H52A,H52B), C54(H54A,H54B), C54(H54C,H54D),
  C55(H55A,H55B), C55A(H55C,H55D), C57(H57A,H57B), C57A(H57C,H57D), C58(H58A,
 H58B), C58(H58C,H58D)
6.c Me refined with riding coordinates:
 C33(H33A,H33B,H33C), C35(H35A,H35B,H35C)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12), C16(H16), C19(H19), C23(H23), C26(H26)
6.e Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C82(H82A,H82B,H82C), C83(H83A,
 H83B,H83C)
;
_shelx_res_checksum              2274