Grafting transition metal-organophosphonate fragments onto heteropolyoxomolybdate: activity in photocatalysis.
Sun, Xiaopeng; Liang, Zhijie; Ma, Pengtao; Ban, Ran; Jiang, Mingshuang; Zhang, Dongdi; Wang, Jingping; Niu, Jingyang; Dalton transactions (Cambridge, England : 2003) 44 (2015) 17544–17550; doi:10.1039/c5dt02471d

data_7036440
_publ_section_title
;
 Grafting transition metal-organophosphonate fragments onto
 heteropolyoxomolybdate: activity in photocatalysis.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17544
_journal_page_last               17550
_journal_paper_doi               10.1039/c5dt02471d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'0.25(C72 H120 Cs4 Mo48 N24 Na36 Ni24 O392 P32), 3(O)'
_chemical_formula_sum            'C18 H86 Cs Mo12 N6 Na9 Ni6 O101 P8'
_chemical_formula_weight         4094.04
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-12 deposited with the CCDC.
2015-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.3710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8247(8)
_cell_length_b                   45.237(2)
_cell_length_c                   18.8324(9)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.38
_cell_volume                     12287.1(10)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0274
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31456
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.482
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.617
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0678 before and 0.0405 after correction.
The Ratio of minimum to maximum transmission is 0.7372.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.213
_exptl_crystal_description       block
_exptl_crystal_F_000             7960
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.893
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         10802
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0808P)^2^+151.9641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8953
_reflns_number_total             10802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02471d2.cif
_cod_data_source_block           njy1
_cod_depositor_comments          'Adding full bibliography for 7036440.cif.'
_cod_original_cell_volume        12287.1(11)
_cod_database_code               7036440
_audit_block_doi                 10.5517/cc14h0xk
_shelx_estimated_absorpt_t_max   0.665
_shelx_estimated_absorpt_t_min   0.354
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2. Rigid bond restraints
 O6W, Na2, Na6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5W, Na5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O7W, Na5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5W, Cs1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O6W \\sim Na2 \\sim Na6: within 2.6A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O5W \\sim Na5: within 2.4A with sigma of 0.01 and sigma for terminal atoms of
0.02
O7W \\sim Na5: within 2.4A with sigma of 0.01 and sigma for terminal atoms of
0.02
O5W \\sim Cs1: within 3.6A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(O7W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: Cs1(0.5) Na3(0.5) Na4(0.5) Na5(0.5) Na6(0.25) Na7(0.5) Na8(0.25)
 O8W(0.5) O9W(0.5) O10W(0.5) O11W(0.25) O12W(0.5) O13W(0.25) O14W(0.5)
 O15W(0.5) O16W(0.5)
 Fixed Uiso: O11W(0.09089) O14W(0.10136) O16W(0.10144)
5.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B)
5.c Aromatic/amide H refined with riding coordinates:
 N3(H3)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'