Microwave-assisted synthesis of organically functionalized hexa-molybdovanadates
Karoui, H.; Ritchie, C.; New Journal of Chemistry 42 (2018) 25–; doi:10.1039/C7NJ02820B

data_7056787
_publ_section_title
;
 Microwave-assisted synthesis of organically functionalized
 hexa-molybdovanadates
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              25
_journal_paper_doi               10.1039/C7NJ02820B
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C5 H9 Mo3 O20 V3, 2(C16 H36 N), C2 H3 N'
_chemical_formula_sum            'C39 H84 Mo3 N3 O20 V3'
_chemical_formula_weight         1355.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-02 deposited with the CCDC.
2017-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.4590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7895(2)
_cell_length_b                   18.8620(3)
_cell_length_c                   18.1257(2)
_cell_measurement_reflns_used    8478
_cell_measurement_temperature    130.00(10)
_cell_measurement_theta_max      74.5410
_cell_measurement_theta_min      4.1570
_cell_volume                     5339.50(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      130.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -49.00  31.00   1.00    2.50    --  -40.81  38.00 -90.00   80
  2  \w     56.00  98.00   1.00    2.50    --   40.81-125.00 -90.00   42
  3  \w     43.00  95.00   1.00    7.50    --  107.94 -45.00-150.00   52
  4  \w     62.00  89.00   1.00    7.50    --  107.94 -30.00 -90.00   27
  5  \w     83.00 173.00   1.00    7.50    --  107.94  30.00-180.00   90
  6  \w     43.00  85.00   1.00    7.50    --  107.94 -45.00  30.00   42
  7  \w     37.00 109.00   1.00    7.50    --  107.94 -94.00  60.00   72
  8  \w     80.00 108.00   1.00    7.50    --  107.94 -94.00 150.00   28
  9  \w     24.00  52.00   1.00    7.50    --  107.94 -94.00 150.00   28
 10  \w     33.00  88.00   1.00    7.50    --  107.94 -30.00 -30.00   55
 11  \w     36.00  76.00   1.00    7.50    --  107.94 -45.00 -90.00   40
 12  \w    152.00 177.00   1.00    7.50    --  107.94 111.00  90.00   25
 13  \w    -96.00 -70.00   1.00    2.50    --  -40.81 125.00  90.00   26
 14  \w   -113.00 -14.00   1.00    2.50    --  -40.81 -57.00 120.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0610135000
_diffrn_orient_matrix_UB_12      -0.0261547000
_diffrn_orient_matrix_UB_13      0.0687784000
_diffrn_orient_matrix_UB_21      -0.0540456000
_diffrn_orient_matrix_UB_22      0.0391720000
_diffrn_orient_matrix_UB_23      0.0513949000
_diffrn_orient_matrix_UB_31      -0.0555302000
_diffrn_orient_matrix_UB_32      -0.0667416000
_diffrn_orient_matrix_UB_33      0.0031986000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22122
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.732
_diffrn_reflns_theta_min         3.401
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.447
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43i (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       rod
_exptl_crystal_F_000             2776
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         10668
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0418P)^2^+3.3214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9257
_reflns_number_total             10668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02820b2.cif
_cod_data_source_block           hk-5-182
_cod_depositor_comments
'Adding full bibliography for 7056787--7056789.cif.'
_cod_database_code               7056787
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         V3Mo3O22C18N2
_chemical_oxdiff_usercomment     'V3Mo3O19(CH2)3CH2OH '
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.62
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Shared sites
{V1, Mo1}
{Mo2, V2}
{Mo3, V3}
{V6, Mo6}
{V5, Mo5}
{V4, Mo4}
3. Restrained distances
 C19-C21
 1.5 with sigma of 0.02
 C21-C20
 1.5 with sigma of 0.02
 C21'-C20'
 1.5 with sigma of 0.02
 C20'-C19'
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Mo1) = Uanis(V1)
Uanis(V2) = Uanis(Mo2)
Uanis(V3) = Uanis(Mo3)
Uanis(Mo4) = Uanis(V4)
Uanis(Mo5) = Uanis(V5)
Uanis(Mo6) = Uanis(V6)
Uanis(C19') = Uanis(C19)
Uanis(C21) = Uanis(C21')
Uanis(C20) = Uanis(C20')
Uanis(V1) = Uanis(Mo1)
Uanis(Mo2) = Uanis(V2)
Uanis(Mo3) = Uanis(V3)
Uanis(V6) = Uanis(Mo6)
Uanis(V5) = Uanis(Mo5)
Uanis(V4) = Uanis(Mo4)
5. Others
 Sof(H18C)=Sof(H18D)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=1-FVAR(1)
 Sof(H18A)=Sof(H18B)=Sof(C19')=Sof(H19C)=Sof(H19D)=Sof(C20')=Sof(H20C)=
 Sof(H20D)=Sof(C21')=Sof(H21D)=Sof(H21E)=Sof(H21F)=FVAR(1)
 Fixed Sof: Mo1(0.5) Mo2(0.25) Mo3(0.25) Mo4(0.75) Mo5(0.5) Mo6(0.75) V1(0.5)
 V2(0.75) V3(0.75) V4(0.25) V5(0.5) V6(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B), C18(H18C,H18D), C19(H19A,H19B),
  C19'(H19C,H19D), C20(H20A,H20B), C20'(H20C,H20D), C22(H22A,H22B), C23(H23A,
 H23B), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C34(H34A,H34B), C35(H35A,H35B),
  C36(H36A,H36B)
6.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C21(H21A,H21B,
 H21C), C21'(H21D,H21E,H21F), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C),
 C33(H33A,H33B,H33C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C)
6.c Idealised tetrahedral OH refined as rotating group:
 O20(H20)
;
_olex2_date_sample_data_collection 2016-12-29
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.524
_oxdiff_exptl_absorpt_empirical_full_min 0.751