Construction of a new binding manner in carboxylic acid-functionalized phosphomolybdates.
Wang, Jin; Shi, Wenjie; Li, Shujie; Mao, Qiyun; Ma, Pengtao; Niu, Jingyang; Wang, Jingping; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7949–7955; doi:10.1039/c8dt01540f

data_7046331
_publ_section_title
;
 Construction of a new binding manner in carboxylic acid-functionalized
 phosphomolybdates.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7949
_journal_page_last               7955
_journal_paper_doi               10.1039/c8dt01540f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C42 H18 Mo36 N6 O156 P8, 6(C4 H12 N), 25(O)'
_chemical_formula_sum            'C66 H140 Mo36 N12 O181 P8'
_chemical_formula_weight         7699.49
_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     direct
_audit_creation_date             2016-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-03-30 deposited with the CCDC.
2018-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                76.6910(10)
_cell_angle_beta                 89.3890(10)
_cell_angle_gamma                71.4410(10)
_cell_formula_units_Z            2
_cell_length_a                   20.9083(14)
_cell_length_b                   24.6633(16)
_cell_length_c                   30.156(2)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      2.24
_cell_volume                     14312.8(16)
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.1042
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            74922
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         0.695
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.652
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0735 before and 0.0402 after correction.
The Ratio of minimum to maximum transmission is 0.7483.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7400
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.301
_refine_diff_density_min         -1.817
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1464
_refine_ls_number_reflns         50682
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1557
_refine_ls_R_factor_gt           0.0834
_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^)+(0.1691P)^2^+63.4408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2423
_refine_ls_wR_factor_ref         0.3095
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27049
_reflns_number_total             50682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01540f2.cif
_cod_data_source_block           njy1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7046330--7046333.cif.'
_cod_original_cell_volume        14313.0(16)
_cod_database_code               7046331
_shelx_estimated_absorpt_t_max   0.755
_shelx_estimated_absorpt_t_min   0.603
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N12-C44 = N12-C49 = N12-C52 = N12-C66
 1.47 with sigma of 0.01
 N10-C43 = N10-C46 = N10-C50 = N10-C53
 1.47 with sigma of 0.01
 N11-C48 = N11-C51 = N11-C56 = N11-C58
 1.47 with sigma of 0.01
 O9-O3W
 2.6 with sigma of 0.01
 C45-C47 \\sim C45-C55 \\sim C45-C59 \\sim C47-C55 \\sim C47-C59 \\sim C55-C59
 with sigma of 0.02
 C44-C49 \\sim C44-C52 \\sim C44-C66 \\sim C49-C52 \\sim C49-C66 \\sim C52-C66
 with sigma of 0.02
 C43-C46 \\sim C43-C50 \\sim C43-C53 \\sim C46-C50 \\sim C46-C53 \\sim C50-C53
 with sigma of 0.02
 C48-C51 \\sim C48-C56 \\sim C48-C58 \\sim C51-C56 \\sim C51-C58 \\sim C56-C58
 with sigma of 0.02
3. Others
 Fixed Sof: O18W(0.5) O19W(0.5) O20W(0.5) O21W(0.5) O22W(0.5) O23W(0.5)
 O24W(0.5) O25W(0.5) O26W(0.5) O27W(0.5) O28W(0.5) O29W(0.5) O30W(0.5)
 O31W(0.5) O32W(0.5) O33W(0.5) O34W(0.5) O35W(0.5) O36W(0.5)
 Fixed Uiso: C43(0.12216) C44(0.12633) C45(0.12367) C47(0.14289) C50(0.1112)
 C66(0.13124)
4.a Me refined with riding coordinates:
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,
 H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C),
 C65(H65A,H65B,H65C), C66(H66A,H66B,H66C)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C11(H11), C15(H15), C18(H18),
 C20(H20), C21(H21), C24(H24), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38),
  C39(H39), C41(H41)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'