Anion complexation, transport and structural studies of a series of bis-methylurea compounds.
Olivari, Martina; Montis, Riccardo; Karagiannidis, Louise E.; Horton, Peter N.; Mapp, Lucy K.; Coles, Simon J.; Light, Mark E.; Gale, Philip A.; Caltagirone, Claudia; Dalton transactions (Cambridge, England : 2003) 44 (2015) 2138–2149; doi:10.1039/c4dt02893g

data_7033743
_publ_section_title
;
 Anion complexation, transport and structural studies of a series of
 bis-methylurea compounds.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2138
_journal_page_last               2149
_journal_paper_doi               10.1039/c4dt02893g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C25 H17 F12 N5 O2'
_chemical_formula_sum            'C25 H17 F12 N5 O2'
_chemical_formula_weight         647.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-11-10 deposited with the CCDC.
2014-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.618(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.210(7)
_cell_length_b                   12.739(3)
_cell_length_c                   8.981(2)
_cell_measurement_reflns_used    3021
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.3
_cell_volume                     2978.7(13)
_computing_cell_refinement       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_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      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
scan:
    Number of images: 111
               Slice: -89.0000 - 22.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: -60.0000
                 XTD: 44.8671
              2theta: -16.8179
scan:
    Number of images: 79
               Slice: -29.0000 - 50.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 72.0000
                 Phi: 60.0000
                 XTD: 44.8671
              2theta: -16.8179
scan:
    Number of images: 20
               Slice: -20.0000 - 0.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: -180.0000
                 XTD: 44.8671
              2theta: -16.8179
scan:
    Number of images: 20
               Slice: -27.0000 - -7.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -18.0000
                 Phi: 60.0000
                 XTD: 44.8671
              2theta: -16.8179
scan:
    Number of images: 61
               Slice: -40.0000 - 21.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 18.0000
                 Phi: 60.0000
                 XTD: 44.8671
              2theta: -16.8179
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.018357
_diffrn_orient_matrix_UB_12      0.030416
_diffrn_orient_matrix_UB_13      0.014599
_diffrn_orient_matrix_UB_21      -0.000392
_diffrn_orient_matrix_UB_22      0.033774
_diffrn_orient_matrix_UB_23      -0.070861
_diffrn_orient_matrix_UB_31      -0.103977
_diffrn_orient_matrix_UB_32      -0.038018
_diffrn_orient_matrix_UB_33      -0.017545
_diffrn_radiation_collimation    0.8
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10448
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         2.823
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3417
_refine_ls_number_restraints     281
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1354P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2513
_reflns_number_total             3417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02893g2.cif
_cod_data_source_block           L4-MeOH
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               7033743
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.970
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 N3-H3 = N2-H2A
 0.88 with sigma of 0.02
3. Rigid bond restraints
 C6, O1, C5, N3, N2, H3, H2A, C4, C7, C11, H11, C10, C3, H4A, H4B, H7, C8, C9,
 C13, N1, C2, C12, F3A, F1, F1A, F3, F2A, F2, H9, F5, F4, F6, F6A, F4A, F5A, C1,
  H2, H1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F1 \\sim F1A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
5. Rigid body (RIGU) restrains
 C8, O1, C5, N3, N2, H3, C6, H2A, C4, C7, C11, C3, H4A, H4B, H7, H11, C10, N1,
 C2, C9, C12, F1, F3, F2, C13, H9, C1, H2, F5, F4, F6, F6A, F4A, F5A, H1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C7(H7), C9(H9), C11(H11)
;
_shelx_res_checksum              66377
_shelx_hkl_checksum              62714
_olex2_submission_special_instructions 'No special instructions were received'