Synthesis of a phosphomolybdate with a tetranuclear vanadium core by installing vanadium atoms in a lacunary template using the protecting group strategy.
Li, Chifeng; Yamaguchi, Kazuya; Suzuki, Kosuke; Chemical communications (Cambridge, England) 57 (2021) 7882–7885; doi:10.1039/d1cc03099j

data_7128638
_publ_section_title
;
 Synthesis of a phosphomolybdate with a tetranuclear vanadium core by
 installing vanadium atoms in a lacunary template using the protecting
 group strategy.
;
_journal_issue                   64
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7882
_journal_page_last               7885
_journal_paper_doi               10.1039/d1cc03099j
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         '1(Mo9 O41 P V4), 2(C16 H36 N), 1(C H2 Cl2)'
_chemical_formula_sum            'C33 H74 Cl2 Mo9 N2 O41 P V4'
_chemical_formula_weight         2324.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-07-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-04 deposited with the CCDC.	2021-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.802(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   55.5617(14)
_cell_length_b                   14.4627(2)
_cell_length_c                   24.0687(6)
_cell_measurement_reflns_used    42449
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.9050
_cell_measurement_theta_min      1.9380
_cell_volume                     17108.3(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       77
_diffrn_reflns_limit_h_min       -80
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            120215
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.143
_diffrn_reflns_theta_min         2.229
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.841
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             9064
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.222
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         25694
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0777
_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^)+(0.0621P)^2^+246.8549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.1867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17091
_reflns_number_total             25694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03099j2.cif
_cod_data_source_block           II
_cod_depositor_comments          'Adding full bibliography for 7128638.cif.'
_cod_original_formula_sum        'C33 H74 Cl2 Mo9 N2 O41 P1 V4'
_cod_database_code               7128638
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.536
_oxdiff_exptl_absorpt_empirical_full_max 1.895
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_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. Uiso/Uaniso restraints and constraints
V2 \\sim O42 \\sim O33 \\sim O34 \\sim O35 \\sim O36: within 1.9A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 1.9A
V106 \\sim O6 \\sim O19 \\sim O20 \\sim O27 \\sim O28: within 1.9A with sigma
of 0.005 and sigma for terminal atoms of 0.01 within 1.9A
V108 \\sim O8 \\sim O23 \\sim O24 \\sim O31 \\sim O32: within 1.9A with sigma
of 0.005 and sigma for terminal atoms of 0.01 within 1.9A
V109 \\sim O8 \\sim O26 \\sim O27 \\sim O33 \\sim O36: within 1.9A with sigma
of 0.001 and sigma for terminal atoms of 0.002 within 1.9A
V110 \\sim O10 \\sim O25 \\sim O33 \\sim O34 \\sim O32: within 1.9A with sigma
of 0.005 and sigma for terminal atoms of 0.01 within 1.9A
V111 \\sim O11 \\sim O30 \\sim O31 \\sim O34 \\sim O35: within 1.9A with sigma
of 0.005 and sigma for terminal atoms of 0.01 within 1.9A
V112 \\sim O12 \\sim O28 \\sim O29 \\sim O35 \\sim O36: within 1.9A with sigma
of 0.005 and sigma for terminal atoms of 0.01 within 1.9A
V101 \\sim O1 \\sim O13 \\sim O16 \\sim O17 \\sim O24: within 1.9A with sigma
of 0.005 and sigma for terminal atoms of 0.01 within 1.9A
Uanis(Mo1) = Uanis(V101)
Uanis(Mo2) = Uanis(V102)
Uanis(Mo3) = Uanis(V103)
Uanis(Mo4) = Uanis(V104)
Uanis(Mo5) = Uanis(V105)
Uanis(Mo6) = Uanis(V106)
Uanis(Mo7) = Uanis(V107)
Uanis(Mo8) = Uanis(V108)
Uanis(Mo9) = Uanis(V109)
Uanis(Mo10) = Uanis(V110)
Uanis(Mo11) = Uanis(V111)
Uanis(Mo12) = Uanis(V112)
3. Others
 Fixed Sof: V1(0.7) O41(0.7) Mo1(0.65) Mo2(0.65) Mo3(0.65) Mo4(0.65) Mo5(0.65)
 Mo7(0.65) V101(0.35) V102(0.35) V103(0.35) V104(0.35) V105(0.35) V107(0.35)
 V2(0.3) O42(0.3) Mo6(0.85) Mo8(0.85) Mo9(0.85) Mo10(0.85) Mo11(0.85)
 Mo12(0.85) V106(0.15) V108(0.15) V109(0.15) V110(0.15) V111(0.15) V112(0.15)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
  C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C51(H51A,H51B), C52(H52A,
 H52B), C53(H53A,H53B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B),
 C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C81(H81A,H81B), C82(H82A,H82B),
  C83(H83A,H83B)
4.b Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C34(H34A,H34B,H34C), C44(H44A,H44B,
 H44C), C54(H54A,H54B,H54C), C64(H64A,H64B,H64C), C74(H74A,H74B,H74C), C84(H84A,
 H84B,H84C)
;
_shelx_res_checksum              60045
_shelx_fab_checksum              28589
_olex2_submission_special_instructions 'No special instructions were received'