Architectural control of urea in supramolecular 1D strontium vanadium oxide chains.
Schwarz, Benjamin; Streb, Carsten; Dalton transactions (Cambridge, England : 2003) 44 (2015) 4195–4199; doi:10.1039/c4dt03691c

data_7033663
_publ_section_title
;
 Architectural control of urea in supramolecular 1D strontium vanadium
 oxide chains.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4195
_journal_page_last               4199
_journal_paper_doi               10.1039/c4dt03691c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'Sr, O14 V5, 4(C3 H7 N O)'
_chemical_formula_sum            'C12 H28 N4 O18 Sr V5'
_chemical_formula_weight         858.70
_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     iterative
_audit_creation_date             2014-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2014-10-05 deposited with the CCDC.
2015-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                104.697(4)
_cell_angle_beta                 99.497(4)
_cell_angle_gamma                109.603(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9593(3)
_cell_length_b                   11.6409(7)
_cell_length_c                   12.2782(7)
_cell_measurement_temperature    150.15
_cell_volume                     1372.51(13)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9.091
_diffrn_detector_type            'Full frame scientific grade 1'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34533
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         6.219
_diffrn_source                   'normal-focus sealed tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    3.646
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0620 before and 0.0418 after correction.
The Ratio of minimum to maximum transmission is 0.7803.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_F_000             850
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.314
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5609
_refine_ls_number_restraints     562
_refine_ls_restrained_S_all      1.338
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+4.0836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5088
_reflns_number_total             5609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03691c2.cif
_cod_data_source_block           p-1
_cod_depositor_comments
'Adding full bibliography for 7033663--7033664.cif.'
_cod_database_code               7033663
_shelxl_version_number           2014-1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O6-C13 \\sim O1-C6 \\sim O3-C4 \\sim O4-C2 \\sim O6-C7
 with sigma of 0.02
 N4-C14 \\sim N2-C6 \\sim N2-C3 \\sim N2-C8 \\sim N1-C4 \\sim N1-C9 \\sim
N1-C10 \\sim N3-C2 \\sim N3-C1 \\sim N3-
 C5 \\sim N4-C7 \\sim N4-C13 \\sim N4-C12 \\sim N4-C11
 with sigma of 0.02
 N4-C15 \\sim N3-C2 \\sim N3-C1 \\sim N3-C5 \\sim N2-C6 \\sim N2-C3 \\sim N2-C8
\\sim N1-C4 \\sim N1-C9 \\sim N1-
 C10 \\sim N4-C7 \\sim N4-C13 \\sim N4-C11 \\sim N4-C12 \\sim N4-C14
 with sigma of 0.02
 O6-C13 \\sim O4-C2 \\sim O1-C6 \\sim O3-C4 \\sim O6-C7
 with sigma of 0.02
 C15-C14 \\sim C12-C11
 with sigma of 0.02
 C15-C13 \\sim C7-C12
 with sigma of 0.02
 C13-C14 \\sim C7-C11
 with sigma of 0.02
 N4-C12 \\sim N2-C6 \\sim N2-C3 \\sim N2-C8 \\sim N1-C4 \\sim N1-C9 \\sim
N1-C10 \\sim N3-C2 \\sim N3-C1 \\sim N3-
 C5 \\sim N4-C7 \\sim N4-C13 \\sim N4-C11 \\sim N4-C14 \\sim N4-C15
 with sigma of 0.05
 N4-C15 \\sim N2-C6 \\sim N2-C3 \\sim N2-C8 \\sim N1-C4 \\sim N1-C9 \\sim
N1-C10 \\sim N3-C2 \\sim N3-C1 \\sim N3-
 C5 \\sim N4-C7 \\sim N4-C13 \\sim N4-C11 \\sim N4-C12 \\sim N4-C14
 with sigma of 0.005
3. Rigid bond restraints
 C7, O6, C13, N4, C12, C14, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15, O6, C7, C13, H7, N4, H13, C11, C12, C14, H11a, H11b, H11c, H14a, H14b,
 H14c
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C7 \\sim O6 \\sim C13 \\sim N4 \\sim C12 \\sim C14 \\sim C11: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C15 \\sim O6 \\sim C7 \\sim C13 \\sim H7 \\sim N4 \\sim H13 \\sim C11 \\sim C12
\\sim C14 \\sim H11a \\sim H11b \\sim H11c \\sim H14a \\sim H14b \\sim H14c:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C13) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(N4) \\sim
Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(C15) \\sim Ueq, : with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C7(0.66667) H7(0.66667) C11(0.66667) H11a(0.66667) H11b(0.66667)
 H11c(0.66667) C12(0.66667) H12a(0.66667) H12b(0.66667) H12c(0.66667)
 C13(0.33333) H13(0.33333) C14(0.33333) H14a(0.33333) H14b(0.33333)
 H14c(0.33333) C15(0.33333) H15a(0.33333) H15b(0.33333) H15c(0.33333)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C13(H13)
6.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C3(H3a,H3b,H3c), C5(H5a,H5b,H5c), C8(H8a,H8b,H8c), C9(H9a,
 H9b,H9c), C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c),
 C14(H14a,H14b,H14c), C15(H15a,H15b,H15c)
;
_shelx_res_checksum              49512