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_7033664
_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         '2(Sr), O28 V10, 4(C H4 N2 O), 5(C3 H7 N O)'
_chemical_formula_sum            'C19 H51 N13 O37 Sr2 V10'
_chemical_formula_weight         1738.36
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-15
_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                90
_cell_angle_beta                 100.681(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8044(5)
_cell_length_b                   23.2995(14)
_cell_length_c                   22.2340(11)
_cell_measurement_temperature    150(2)
_cell_volume                     5500.1(5)
_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      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 0.984
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38057
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.501
_diffrn_reflns_theta_min         6.235
_diffrn_source                   'normal-focus sealed tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    3.644
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0725 before and 0.0471 after correction.
The Ratio of minimum to maximum transmission is 0.8461.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    2.099
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 4713 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0033(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         10852
_refine_ls_number_restraints     652
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0198
_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^)+(0.0226P)^2^+4.3025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0467
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                10292
_reflns_number_total             10852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03691c2.cif
_cod_data_source_block           cc
_cod_depositor_comments
'Adding full bibliography for 7033663--7033664.cif.'
_cod_database_code               7033664
_shelxl_version_number           2014-1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C40) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C40) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C23(H23), C8(H8), C3(H3), C5(H5)
4.b X=CH2 refined with riding coordinates:
 N1(H1a,H1b), N3(H3a,H3b), N4(H4d,H4e), N5(H5a,H5b), N7(H7d,H7e), N8(H8a,H8b),
 N6(H6d,H6e), N9(H9d,H9e)
4.c Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c), C22(H22a,H22b,H22c), C27(H27a,H27b,H27c), C40(H40a,H40b,
 H40c), C2(H2a,H2b,H2c), C13(H13a,H13b,H13c), C7(H7a,H7b,H7c), C4(H4a,H4b,H4c),
 C6(H6a,H6b,H6c), C9(H9a,H9b,H9c)
;
_shelx_res_checksum              60642