Hydrate smaller than the anhydrate
Zieliński, Witold; Katrusiak, Andrzej; CrystEngComm 17 (2015) 5468–; doi:10.1039/C5CE00694E

data_7220636
_publ_section_title
;
 Hydrate smaller than the anhydrate
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              5468
_journal_paper_doi               10.1039/C5CE00694E
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         '0.25(H4 O4), 2(C9 H10 N2)'
_chemical_formula_sum            'C18 H21 N4 O'
_chemical_formula_weight         309.39
_chemical_name_systematic        Xcalibur
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-28 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.5684(10)
_cell_length_b                   12.432(2)
_cell_length_c                   34.803(4)
_cell_measurement_reflns_used    614
_cell_measurement_temperature    296
_cell_measurement_theta_max      19.8710
_cell_measurement_theta_min      4.6730
_cell_volume                     3274.6(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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      296
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_details
;
  1 omega  -92.00  -66.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -        1.7187 -178.0000    0.0000 26

  2 omega  -73.00  -45.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -        1.7187 -178.0000 -180.0000 28

  3 omega  -63.00  -37.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -        1.7187 -178.0000    0.0000 26

  4 omega  -18.00   45.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.7209   77.0000   30.0000 63

  5 omega -118.00  -92.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.7209  -99.0000  -30.0000 26

  6 omega  -49.00   56.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       31.1584  -38.0000  150.0000 105

  7 omega -103.00  -35.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -        1.7187 -178.0000 -120.0000 68

  8 omega  -47.00   92.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -        1.7187   61.0000  -62.0000 139

  9 omega  -20.00  121.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       31.1584   77.0000   90.0000 141
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0039645000
_diffrn_orient_matrix_UB_12      -0.0407343000
_diffrn_orient_matrix_UB_13      0.0142343000
_diffrn_orient_matrix_UB_21      -0.0317546000
_diffrn_orient_matrix_UB_22      0.0369330000
_diffrn_orient_matrix_UB_23      0.0139297000
_diffrn_orient_matrix_UB_31      -0.0880518000
_diffrn_orient_matrix_UB_32      -0.0151858000
_diffrn_orient_matrix_UB_33      -0.0043740000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1387
_diffrn_reflns_av_unetI/netI     0.1362
_diffrn_reflns_laue_measured_fraction_full 0.969
_diffrn_reflns_laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            3718
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.522
_diffrn_reflns_theta_min         4.302
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.200
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1719
_refine_ls_R_factor_gt           0.0772
_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^)+(0.0633P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1999
_reflns_Friedel_coverage         0.000
_reflns_number_gt                389
_reflns_number_total             798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00694e2.cif
_cod_data_source_block           dMBzImH_AP
_cod_depositor_comments
'Adding full bibliography for 7220631--7220640.cif.'
_cod_original_cell_volume        3274.5(8)
_cod_database_code               7220636
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: H1(0.25) H3(0.5)
3.a Free rotating group:
 O1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C2(H2), C4(H4)
3.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_shelx_res_checksum              75540
_olex2_submission_special_instructions 'No special instructions were received'