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

data_7056789
_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
'C4 H8 Mo3 N O19 V3, C16 H36 N, C16 H35 N, C2 H3 N'
_chemical_formula_sum            'C38 H82 Mo3 N4 O19 V3'
_chemical_formula_weight         1339.71
_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   mixed
_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                 100.088(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7948(3)
_cell_length_b                   18.5129(3)
_cell_length_c                   18.2430(3)
_cell_measurement_reflns_used    12114
_cell_measurement_temperature    130.00(10)
_cell_measurement_theta_max      75.3090
_cell_measurement_theta_min      4.7020
_cell_volume                     5251.92(16)
_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      N~2~
_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 0.999
_diffrn_measured_fraction_theta_max 0.979
_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    -48.00  35.00   1.00    5.00    --  -40.81  38.00 120.00   83
  2  \w    -38.00  74.00   1.00    5.00    --   40.81 -77.00-120.00  112
  3  \w     23.00  95.00   1.00    5.00    --   40.81-125.00-180.00   72
  4  \w     44.00 115.00   1.00   10.00    --  110.21-111.00 -60.00   71
  5  \w     46.00 144.00   1.00   10.00    --  110.21 -77.00 -60.00   98
  6  \w     50.00 175.00   1.00   10.00    --  110.21  15.00-120.00  125
  7  \w     80.00 174.00   1.00   10.00    --  110.21  61.00 -90.00   94
  8  \w     32.00  91.00   1.00   10.00    --  110.21 -30.00 -60.00   59
  9  \w     36.00  91.00   1.00   10.00    --  110.21 -30.00-120.00   55
 10  \w     32.00 115.00   1.00   10.00    --  110.21-111.00 120.00   83
 11  \w     31.00 144.00   1.00   10.00    --  110.21 -77.00 120.00  113
 12  \w   -115.00 -13.00   1.00    5.00    --  -40.81 -57.00 -30.00  102
;
_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      0.0669563000
_diffrn_orient_matrix_UB_12      -0.0317670000
_diffrn_orient_matrix_UB_13      -0.0431013000
_diffrn_orient_matrix_UB_21      0.0527903000
_diffrn_orient_matrix_UB_22      -0.0281624000
_diffrn_orient_matrix_UB_23      0.0735246000
_diffrn_orient_matrix_UB_31      -0.0504402000
_diffrn_orient_matrix_UB_32      -0.0715589000
_diffrn_orient_matrix_UB_33      -0.0097783000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32619
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.787
_diffrn_reflns_theta_min         3.428
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.605
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54942
_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_density_diffrn    1.694
_exptl_crystal_F_000             2740
_refine_diff_density_max         1.410
_refine_diff_density_min         -1.696
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         10711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0693
_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^)+(0.0869P)^2^+88.6063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2428
_refine_ls_wR_factor_ref         0.2465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9429
_reflns_number_total             10711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02820b2.cif
_cod_data_source_block           hk-5-164-amine
_cod_depositor_comments
'Adding full bibliography for 7056787--7056789.cif.'
_cod_database_code               7056789
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         V3Mo3C22N3O20
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{V6, Mo6}
{Mo1, V1}
{Mo2, V2}
{V4, Mo4}
{V3, Mo3}
{V5, Mo5}
3. Uiso/Uaniso restraints and constraints
Uanis(Mo3) = Uanis(V3)
Uanis(Mo5) = Uanis(V5)
Uanis(Mo6) = Uanis(V6)
Uanis(Mo4) = Uanis(V4)
Uanis(V6) = Uanis(Mo6)
Uanis(Mo1) = Uanis(V1)
Uanis(Mo2) = Uanis(V2)
Uanis(V4) = Uanis(Mo4)
Uanis(V3) = Uanis(Mo3)
Uanis(V5) = Uanis(Mo5)
4. Others
 Fixed Sof: Mo1(0.25) Mo2(0.5) Mo3(0.25) Mo4(0.5) Mo5(0.75) Mo6(0.75) V1(0.75)
 V2(0.5) V3(0.75) V4(0.5) V5(0.25) V6(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1C,H1D), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C22(H22A,H22B),
  C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C20(H20A,H20B,
 H20C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C)
;
_olex2_date_sample_data_collection 2017-03-16
_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 2.191
_oxdiff_exptl_absorpt_empirical_full_min 0.474