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_7220279
_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         'C44 H54 O11, C2 H3 N'
_chemical_formula_sum            'C46 H57 N O11'
_chemical_formula_weight         799.93
_chemical_name_common
'C-methyl tetramethoxy resorcinarene mono-crown-5 acetonitrilesolvate'
_chemical_name_systematic
'C-methyl tetramethoxy resorcinarene mono-crown-5 acetonitrile solvate'
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-25
_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                90.00
_cell_angle_beta                 114.831(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5554(3)
_cell_length_b                   13.43772(18)
_cell_length_c                   19.9408(4)
_cell_measurement_reflns_used    7520
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0584
_cell_measurement_theta_min      3.1911
_cell_volume                     4269.23(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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      173.0
_diffrn_detector_area_resol_mean 16.0107
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
  1 omega   -3.00   84.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3796   57.0000  150.0000 87

  2 omega  -53.00   34.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3796  -57.0000    0.0000 87
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0240919000
_diffrn_orient_matrix_UB_12      0.0438608000
_diffrn_orient_matrix_UB_13      -0.0135845000
_diffrn_orient_matrix_UB_21      0.0271168000
_diffrn_orient_matrix_UB_22      0.0147102000
_diffrn_orient_matrix_UB_23      -0.0163688000
_diffrn_orient_matrix_UB_31      -0.0258041000
_diffrn_orient_matrix_UB_32      -0.0254553000
_diffrn_orient_matrix_UB_33      -0.0329083000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0159
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14501
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.23
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         8041
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0441P)^2^+2.2728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                6628
_reflns_number_total             8041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00311c2.cif
_cod_data_source_block           2-II
_cod_depositor_comments
'Adding full bibliography for 7220270--7220279.cif.'
_cod_original_cell_volume        4269.23(13)
_cod_database_code               7220279
_chemical_oxdiff_formula         'C46 H57 O11 N1'
_reflns_odcompleteness_completeness 98.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O25-H25 = O18-H18
 0.82 with sigma of 0.02
 N100-C101 = N104-C103
 1.16 with sigma of 0.02
 C101-C102 = C105-C103
 1.54 with sigma of 0.02
3. Rigid bond restraints
 N100, C101, C102
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C105, C103, N104
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N100 \\sim C101 \\sim C102: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C105 \\sim C103 \\sim N104: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C101) = Uanis(N100)
Uanis(C102) = Uanis(C105)
5. Others
 Sof(N104)=Sof(C103)=Sof(C105)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(N100)=Sof(C101)=Sof(C102)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C28(H28), C21(H21), C14(H14), C7(H7)
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)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C23(H23), C26(H26), C16(H16), C19(H19), C9(H9), C12(H12)
6.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C29(H29A,H29B,
 H29C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C34(H34A,
 H34B,H34C), C102(H10A,H10B,H10C), C105(H10D,H10E,H10F)
;
_shelx_res_checksum              96494