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_7033747
_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
'2(C25 H17 F12 N5 O2), 2(C16 H36 N), H O4 P, C2 H6 O S'
_chemical_formula_sum            'C84 H113 F24 N12 O9 P S'
_chemical_formula_weight         1953.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_audit_update_record
;
2014-11-10 deposited with the CCDC.
2014-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.732(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5362(16)
_cell_length_b                   32.550(4)
_cell_length_c                   23.279(3)
_cell_measurement_reflns_used    12429
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.0
_cell_volume                     9413(2)
_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 2.1 b29 (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 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
scan:
    Number of images: 228
               Slice: -109.0000 - 5.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: -36.0000
                 XTD: 49.9605
              2theta: -18.8271
scan:
    Number of images: 194
               Slice: -75.0000 - 22.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: 108.0000
                 XTD: 49.9605
              2theta: -18.8271
scan:
    Number of images: 196
               Slice: -49.0000 - 49.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 72.0000
                 Phi: -36.0000
                 XTD: 49.9605
              2theta: -18.8271
scan:
    Number of images: 40
               Slice: -109.0000 - -89.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: -180.0000
                 XTD: 49.9605
              2theta: -18.8271
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_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      0.076304
_diffrn_orient_matrix_UB_12      0.025481
_diffrn_orient_matrix_UB_13      0.002967
_diffrn_orient_matrix_UB_21      0.003138
_diffrn_orient_matrix_UB_22      -0.005906
_diffrn_orient_matrix_UB_23      -0.029985
_diffrn_orient_matrix_UB_31      -0.007439
_diffrn_orient_matrix_UB_32      0.041749
_diffrn_orient_matrix_UB_33      -0.009002
_diffrn_radiation_collimation    0.3
_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  0.0703
_diffrn_reflns_av_unetI/netI     0.0847
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            66676
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_min         1.964
_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    0.159
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.715
_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    1.379
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1280
_refine_ls_number_reflns         21529
_refine_ls_number_restraints     407
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0972P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.2000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11787
_reflns_number_total             21529
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02893g2.cif
_cod_data_source_block           L4-HPO42-(2:1)
_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               7033747
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.967
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F2-C14 = F3A-C14 = F3-C14 = F2A-C14 = F1A-C14 = F1-C14
 1.3 with sigma of 0.02
 F2A-F3A
 2.1 with sigma of 0.02
 F1A-F2A
 2.1 with sigma of 0.02
 F1A-F3A
 2.1 with sigma of 0.02
 F2-F3
 2.1 with sigma of 0.02
 F3-F1
 2.1 with sigma of 0.02
 F1-F2
 2.1 with sigma of 0.02
 N5-H5 = N4-H4A = N2-H2A = N3-H3A = N35-H35 = N34-H34A = N32-H32A = N33-H33A
 0.88 with sigma of 0.02
 F2-C14 = F3-C14
 1.3 with sigma of 0.002
 F2A-C14
 1.3 with sigma of 0.02
 F1A-C14A = F2-C14 = F3A-C14A = F3-C14 = F1-C14 = F2A-C14A
 1.3 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(F39) = Uanis(F39A)
Uanis(F42) = Uanis(F42A)
Uanis(F40) = Uanis(F40A)
Uanis(F41) = Uanis(F41A)
Uanis(F37) = Uanis(F37A)
Uanis(F38) = Uanis(F38A)
Uanis(F12) = Uanis(F12A)
Uanis(F10) = Uanis(F10A)
Uanis(F11) = Uanis(F11A)
Uanis(F42) = Uanis(F40A)
Uanis(F41) = Uanis(F42A)
4. Rigid body (RIGU) restrains
 C14, O2, C17, N4, N5, H4A, C16, H5, C18, C1, H16A, H16B, C23, C19, N1, C2,
 H23, C22, H19, C20, C5, C3, H2, C21, C25, C24, C6, C4, H3, H21, F7, F9, F8,
 F11, F10, F12, N2, H6A, H6B, H4, H2A, C7, N3, O1, H3A, C8, C13, C9, H13, C12,
 H9, C10, C15, C11, F6, F5, F4, H11, F1A, F2A, F3A, F3, F2, F1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, C14A, F3A, F2, F3, F1A, F2A, F1, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F1)=Sof(F2)=Sof(F3)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(1)
 Sof(F10A)=Sof(F12A)=Sof(F11A)=1-FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
 Sof(F37A)=Sof(F38A)=Sof(F39A)=1-FVAR(3)
 Sof(F37)=Sof(F38)=Sof(F39)=FVAR(3)
 Sof(F42A)=Sof(F41A)=Sof(F40A)=1-FVAR(4)
 Sof(F40)=Sof(F41)=Sof(F42)=FVAR(4)
 Sof(C14A)=1-FVAR(5)
 Sof(C14)=FVAR(5)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C16(H16A,H16B), C36(H36A,H36B), C46(H46A,H46B), C71(H71A,H71B),
 C72(H72A,H72B), C73(H73A,H73B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B),
  C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C83(H83A,H83B), C84(H84A,
 H84B), C85(H85A,H85B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B),
 C95(H95A,H95B), C96(H96A,H96B), C97(H97A,H97B), C99(H99A,H99B), C100(H10A,
 H10B), C101(H10C,H10D), C103(H10H,H10I), C104(H10J,H10K), C105(H10L,H10M)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C9(H9), C11(H11), C13(H13), C19(H19), C21(H21),
 C23(H23), C32(H32), C33(H33), C34(H34), C39(H39), C41(H41), C43(H43), C49(H49),
  C51(H51), C53(H53)
6.c Idealised Me refined as rotating group:
 C74(H74A,H74B,H74C), C78(H78A,H78B,H78C), C82(H82A,H82B,H82C), C86(H86A,H86B,
 H86C), C94(H94A,H94B,H94C), C98(H98A,H98B,H98C), C102(H10E,H10F,H10G),
 C106(H10N,H10O,H10P), C111(H11A,H11B,H11C), C112(H11D,H11E,H11F)
;
_shelx_res_checksum              13055
_shelx_hkl_checksum              3585
_olex2_submission_special_instructions 'No special instructions were received'