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

data_7056788
_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         'C7 H11 Mo3 O21 V3'
_chemical_formula_sum            'C39 H83 Mo3 N2 O21 V3'
_chemical_formula_weight         1356.71
_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     dual
_audit_creation_date             2017-06-02
_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                90.952(6)
_cell_angle_beta                 93.807(5)
_cell_angle_gamma                91.862(5)
_cell_formula_units_Z            8
_cell_length_a                   21.4889(13)
_cell_length_b                   22.7196(17)
_cell_length_c                   24.1556(17)
_cell_measurement_reflns_used    4129
_cell_measurement_temperature    130.00(10)
_cell_measurement_theta_max      70.5900
_cell_measurement_theta_min      4.0680
_cell_volume                     11758.9(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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   -115.00 -11.00   1.00   10.00    --  -40.81 -57.00  90.00  104
  2  \w    -50.00  35.00   1.00   10.00    --  -40.81  38.00-120.00   85
  3  \w    -96.00  -2.00   1.00   10.00    --  -40.81 125.00 -60.00   94
  4  \w     77.00 173.00   1.00   30.00    --  106.63  30.00   0.00   96
  5  \w    134.00 178.00   1.00   30.00    --  106.63  61.00 -60.00   44
  6  \w     41.00 121.00   1.00   30.00    --  106.63-125.00   0.00   80
  7  \w     35.00 121.00   1.00   30.00    --  106.63-125.00 150.00   86
  8  \w     76.00 172.00   1.00   30.00    --  106.63  61.00-150.00   96
  9  \w     80.00 178.00   1.00   30.00    --  106.63  45.00 -90.00   98
 10  \w     78.00 112.00   1.00   30.00    --  106.63  61.00 -60.00   34
 11  \w     28.00 140.00   1.00   30.00    --  106.63 -77.00 150.00  112
 12  \w     32.00 118.00   1.00   30.00    --  106.63 -61.00 -30.00   86
;
_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      0.0261578000
_diffrn_orient_matrix_UB_12      -0.0504428000
_diffrn_orient_matrix_UB_13      -0.0339398000
_diffrn_orient_matrix_UB_21      -0.0235859000
_diffrn_orient_matrix_UB_22      -0.0448756000
_diffrn_orient_matrix_UB_23      0.0415819000
_diffrn_orient_matrix_UB_31      -0.0626713000
_diffrn_orient_matrix_UB_32      -0.0067868000
_diffrn_orient_matrix_UB_33      -0.0347271000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0934
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43456
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        50.435
_diffrn_reflns_theta_max         50.435
_diffrn_reflns_theta_min         3.510
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.497
_exptl_absorpt_correction_T_max  0.591
_exptl_absorpt_correction_T_min  0.462
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       block
_exptl_crystal_F_000             5552
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.417
_refine_diff_density_min         -1.934
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.281
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         24359
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.283
_refine_ls_R_factor_all          0.1909
_refine_ls_R_factor_gt           0.1501
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3839
_refine_ls_wR_factor_ref         0.4348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12691
_reflns_number_total             24359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02820b2.cif
_cod_data_source_block           hk-6-42
_cod_depositor_comments
'Adding full bibliography for 7056787--7056789.cif.'
_cod_database_code               7056788
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         V3Mo3O22C38H83N2
_reflns_odcompleteness_completeness 98.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Mo2, V2}
{V1, Mo1}
{V3, Mo3}
{V5, Mo5}
{V6, Mo6}
{V4, Mo4}
{Mo9, V9}
{V8, Mo8}
{Mo7, V7}
{Mo11, V11}
{Mo12, V12}
{Mo10, V10}
{V20, Mo20}
{Mo22, V22}
{Mo24, V24}
{V23, Mo23}
{V19, Mo19}
{Mo21, V21}
{V14, Mo14}
{V18, Mo18}
{V17, Mo17}
{V13, Mo13}
{V15, Mo15}
{V16, Mo16}
3. Restrained distances
 C27-O84
 1.22 with sigma of 0.02
 C27-C28
 1.45 with sigma of 0.02
 C28-C27
 1.45 with sigma of 0.01
 Mo13-O43
 2 with sigma of 0.02
 Mo18-O43
 2 with sigma of 0.02
 C15-O41
 1.4 with sigma of 0.02
 Mo18-O52
 2 with sigma of 0.02
 O52-Mo17
 2 with sigma of 0.02
 O84-O83
 2.3 with sigma of 0.04
 O83-C28
 2.35 with sigma of 0.04
 O84-C28
 2.35 with sigma of 0.04
4. Restrained planarity
 O83, O84, C27, C28
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(V2) = Uanis(Mo2)
Uanis(Mo2) = Uanis(V2)
Uanis(V1) = Uanis(Mo1)
Uanis(V3) = Uanis(Mo3)
Uanis(Mo6) = Uanis(V6)
Uanis(Mo4) = Uanis(V4)
Uanis(Mo5) = Uanis(V5)
Uanis(V5) = Uanis(Mo5)
Uanis(V6) = Uanis(Mo6)
Uanis(V4) = Uanis(Mo4)
Uanis(Mo8) = Uanis(V8)
Uanis(Mo9) = Uanis(V9)
Uanis(V8) = Uanis(Mo8)
Uanis(Mo7) = Uanis(V7)
Uanis(Mo11) = Uanis(V11)
Uanis(Mo12) = Uanis(V12)
Uanis(Mo10) = Uanis(V10)
Uanis(Mo23) = Uanis(V23)
Uanis(Mo19) = Uanis(V19)
Uanis(Mo20) = Uanis(V20)
Uanis(V20) = Uanis(Mo20)
Uanis(Mo22) = Uanis(V22)
Uanis(Mo24) = Uanis(V24)
Uanis(V23) = Uanis(Mo23)
Uanis(V19) = Uanis(Mo19)
Uanis(Mo21) = Uanis(V21)
Uanis(Mo17) = Uanis(V17)
Uanis(Mo18) = Uanis(V18)
Uanis(Mo13) = Uanis(V13)
Uanis(Mo14) = Uanis(V14)
Uanis(Mo15) = Uanis(V15)
Uanis(Mo16) = Uanis(V16)
Uanis(V14) = Uanis(Mo14)
Uanis(V18) = Uanis(Mo18)
Uanis(V17) = Uanis(Mo17)
Uanis(V13) = Uanis(Mo13)
Uanis(V15) = Uanis(Mo15)
Uanis(V16) = Uanis(Mo16)
6. Others
 Fixed Sof: Mo1(0.25) Mo2(0.5) Mo3(0.25) Mo4(0.75) Mo5(0.5) Mo6(0.75) V1(0.75)
 V2(0.5) V3(0.75) V4(0.25) V5(0.5) V6(0.25) Mo7(0.5) Mo8(0.25) Mo9(0.25)
 Mo10(0.75) Mo11(0.75) Mo12(0.5) V7(0.5) V8(0.75) V9(0.75) V10(0.25) V11(0.25)
 V12(0.5) Mo13(0.5) Mo14(0.5) Mo15(0.5) Mo16(0.5) Mo17(0.5) Mo18(0.5) V13(0.5)
 V14(0.5) V15(0.5) V16(0.5) V17(0.5) V18(0.5) Mo19(0.5) Mo20(0.5) Mo21(0.5)
 Mo22(0.5) Mo23(0.5) Mo24(0.5) V19(0.5) V20(0.5) V21(0.5) V22(0.5) V23(0.5)
 V24(0.5)
 Fixed Uiso: O39(0.1) O40(0.1) O41(0.1) O42(0.1) O43(0.1) O47(0.1) O49(0.1)
 O50(0.1) O51(0.1) O52(0.1) O53(0.07) O55(0.1) O57(0.07) O81(0.1) O82(0.1)
 C15(0.1) C16(0.1) C17(0.1) C18(0.1) C19(0.1) C20(0.1) C21(0.1) O83(0.1)
 O84(0.1) C22(0.1) C23(0.1) C24(0.1) C25(0.1) C26(0.1) C27(0.1) C28(0.1)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B), C12(H12A,H12B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
  C19(H19A,H19B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B)
7.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C)
;
_olex2_date_sample_data_collection 2017-02-13
_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 1.688
_oxdiff_exptl_absorpt_empirical_full_min 0.559