A hybrid polyoxometalate-organic molecular catalyst for visible light driven water oxidation
C. Zhang; X. Lin; Z. Zhang; L.-S. Long; C. Wang; W. Lin; Chem.Commun. 50 (2014) 11591–; doi:10.1039/C4cc03487B

data_7115682
_publ_section_title
;
 A hybrid polyoxometalate-organic molecular catalyst for visible light
 driven water oxidation
;
_journal_name_full               Chem.Commun.
_journal_page_first              11591
_journal_paper_doi               10.1039/C4cc03487B
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety
'C20 H16 Co2 Mo12 N4 O40 P, C15 H9 Co1.5 Mo12 N3 O40 P, 3(C30 H24 Co N6), 4.5(O), C5 N'
_chemical_formula_sum            'C130 H97 Co6.5 Mo24 N26 O88 P2'
_chemical_formula_weight         6178.88
_chemical_name_systematic
;
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.178(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.607(4)
_cell_length_b                   26.660(3)
_cell_length_c                   24.133(3)
_cell_measurement_reflns_used    7361
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.73
_cell_measurement_theta_min      2.25
_cell_volume                     18098(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXH-1997 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'image plate detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0896
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            91307
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.72
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.294
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11906
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.891
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2497
_refine_ls_number_reflns         31824
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0895P)^2^+94.4085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1732
_refine_ls_wR_factor_ref         0.1866
_reflns_number_gt                22521
_reflns_number_total             31824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc03487b2.cif
_cod_data_source_block           1
_cod_original_cell_volume        18097(4)
_cod_original_formula_sum        'C130 H97 Co6.50 Mo24 N26 O88 P2'
_cod_database_code               7115682
_olex2_refinement_description
;
1. Shared sites
{C34A, N7A}
{C34, N7}
2. Others
 Fixed Sof: Co4(0.5) O1W(0.5) O2W(0.5) O3W(0.5) O5W(0.5) O6W(0.5) O7W(0.5)
 O8W(0.5) N7A(0.5) N7(0.5) C34(0.5) C34A(0.5)
 Fixed Uiso: H1(0.062) H2(0.078) H3(0.077) H4(0.062) H7(0.072) H8(0.078)
 H9(0.078) H10(0.061) H11(0.081) H12(0.089) H13(0.09) H14(0.088) H17(0.101)
 H18(0.139) H19(0.123) H20(0.082) H21(0.053) H22(0.065) H23(0.067) H24(0.062)
 H27(0.058) H28(0.075) H29(0.062) H30(0.055) H32(0.098) H36(0.05) H37(0.046)
 H38(0.045) H39(0.039) H42(0.044) H43(0.053) H44(0.045) H45(0.041) H46(0.041)
 H47(0.056) H48(0.067) H49(0.057) H52(0.053) H53(0.071) H54(0.063) H55(0.049)
 H56(0.076) H57(0.082) H58(0.082) H59(0.063) H62(0.053) H63(0.057) H64(0.064)
 H65(0.057) H66(0.044) H67(0.05) H68(0.06) H69(0.057) H72(0.06) H73(0.062)
 H74(0.048) H75(0.037) H76(0.045) H77(0.058) H78(0.059) H79(0.048) H82(0.06)
 H83(0.068) H84(0.067) H85(0.052) H86(0.046) H87(0.068) H88(0.084) H89(0.076)
 H92(0.05) H93(0.044) H94(0.045) H95(0.039) H96(0.091) H97(0.093) H98(0.1)
 H99(0.091) H102(0.213) H103(0.262) H104(0.181) H105(0.154) H106(0.245)
 H107(0.233) H108(0.249) H110(0.243) H112(0.171) H113(0.209) H114(0.201)
 H115(0.157) H116(0.091) H117(0.098) H118(0.104) H119(0.091) H122(0.087)
 H123(0.108) H124(0.104) H125(0.098)
 Fixed X: H1(-0.288) H2(-0.2465) H3(-0.2311) H4(-0.2507) H7(-0.2697) H9(-
 0.3306) H10(-0.3426) H11(-0.5445) H12(-0.6098) H13(-0.6004) H14(-0.5285) H17(-
 0.4621) H18(-0.3876) H19(-0.3286) H20(-0.3494) H21(-0.7658) H22(-0.738) H23(-
 0.7146) H24(-0.7224) H27(-0.7336) H28(-0.7447) H29(-0.7721) H30(-0.7949) H32(-
 0.8672) H36(-0.073) H37(-0.0146) H38(0.0538) H39(0.0615) H42(0.0618)
 H43(0.0603) H44(0.001) H45(-0.0592) H46(-0.0006) H47(0.0397) H48(0.015) H49(-
 0.0498) H52(-0.1151) H53(-0.1781) H54(-0.2035) H55(-0.1674) H56(-0.101) H57(-
 0.1513) H58(-0.2152) H59(-0.2264) H62(-0.2389) H63(-0.2407) H64(-0.1747) H65(-
 0.1129) H66(-0.0682) H67(-0.0781) H68(-0.1541) H69(-0.2193) H72(-0.2759) H73(-
 0.3323) H74(-0.3067) H75(-0.2277) H76(-0.1252) H77(-0.1219) H78(-0.127) H79(-
 0.1307) H82(-0.146) H83(-0.1593) H84(-0.1523) H85(-0.1378) H86(-0.187) H87(-
 0.1717) H88(-0.0947) H89(-0.0334) H92(0.0206) H93(0.0739) H94(0.0462) H95(-
 0.0324) H96(-0.5265) H97(-0.4464) H98(-0.4196) H99(-0.4722) H102(-0.5254)
 H103(-0.5864) H104(-0.6638) H105(-0.6777) H106(-0.608) H107(-0.6159) H108(-
 0.6235) H110(-0.6166) H112(-0.6116) H113(-0.614) H114(-0.6166) H115(-0.6233)
 H116(-0.5584) H117(-0.5704) H118(-0.6491) H119(-0.7107) H122(-0.7631) H123(-
 0.8181) H124(-0.7885) H125(-0.7103)
 Fixed Y: H1(0.8927) H2(0.9647) H3(1.0253) H4(1.0076) H7(0.9867) H9(0.8793)
 H10(0.8331) H11(0.5803) H12(0.5425) H13(0.462) H14(0.4185) H17(0.3852)
 H18(0.3545) H19(0.4057) H20(0.4848) H21(0.8599) H22(0.9188) H23(0.9955)
 H24(1.015) H27(1.027) H28(1.0354) H29(0.9662) H30(0.8959) H32(0.4179)
 H36(0.6997) H37(0.7593) H38(0.7426) H39(0.6661) H42(0.5938) H43(0.5153)
 H44(0.459) H45(0.4891) H46(0.6114) H47(0.5771) H48(0.5006) H49(0.4606)
 H52(0.4316) H53(0.4007) H54(0.445) H55(0.5182) H56(0.5893) H57(0.6253)
 H58(0.6717) H59(0.6803) H62(0.674) H63(0.6811) H64(0.6517) H65(0.6151)
 H66(0.6803) H67(0.7198) H68(0.7339) H69(0.7078) H72(0.6715) H73(0.6347)
 H74(0.5943) H75(0.5926) H76(0.6084) H77(0.5414) H78(0.4612) H79(0.4475)
 H82(0.4398) H83(0.4382) H84(0.5118) H85(0.5855) H86(0.7025) H87(0.7503)
 H88(0.7634) H89(0.7283) H92(0.7001) H93(0.6537) H94(0.5936) H95(0.5785)
 H96(0.8483) H97(0.8296) H98(0.7773) H99(0.7379) H102(0.7208) H103(0.6981)
 H104(0.7236) H105(0.7616) H106(0.8565) H107(0.9416) H108(1.0121) H110(1.0037)
 H112(0.9854) H113(0.9632) H114(0.8828) H115(0.8203) H116(0.7347) H117(0.6663)
 H118(0.6432) H119(0.6922) H122(0.7471) H123(0.7998) H124(0.8594) H125(0.8648)
 Fixed Z: H1(-0.0625) H2(-0.0212) H3(-0.0831) H4(-0.1811) H7(-0.2728) H9(-
 0.392) H10(-0.317) H11(-0.1185) H12(-0.0999) H13(-0.0627) H14(-0.0456) H17(-
 0.0382) H18(-0.0246) H19(-0.0409) H20(-0.075) H21(-0.225) H22(-0.1508) H23(-
 0.1742) H24(-0.2704) H27(-0.3639) H28(-0.4606) H29(-0.521) H30(-0.4826) H32(-
 0.4812) H36(0.181) H37(0.2066) H38(0.2833) H39(0.3287) H42(0.3727) H43(0.4089)
 H44(0.3591) H45(0.28) H46(0.1567) H47(0.1003) H48(0.0572) H49(0.0721)
 H52(0.0862) H53(0.1126) H54(0.1805) H55(0.2158) H56(0.3289) H57(0.3736)
 H58(0.317) H59(0.2183) H62(0.1241) H63(0.0279) H64(0.0035) H65(0.0737) H66(-
 0.3123) H67(-0.3984) H68(-0.4609) H69(-0.4321) H72(-0.4061) H73(-0.3704) H74(-
 0.2824) H75(-0.2312) H76(-0.1126) H77(-0.0498) H78(-0.0855) H79(-0.1807) H82(-
 0.2755) H83(-0.373) H84(-0.4217) H85(-0.3705) H86(-0.1932) H87(-0.11) H88(-
 0.0545) H89(-0.0791) H92(-0.1165) H93(-0.1495) H94(-0.2173) H95(-0.2553) H96(-
 0.0487) H97(-0.0114) H98(0.0663) H99(0.1038) H102(0.1431) H103(0.1876)
 H104(0.1317) H105(0.0451) H106(0.1041) H107(0.1357) H108(0.078) H110(-0.0096)
 H112(-0.0997) H113(-0.1939) H114(-0.2173) H115(-0.1568) H116(-0.0639) H117(-
 0.1256) H118(-0.1785) H119(-0.1625) H122(-0.1571) H123(-0.1365) H124(-0.0607)
 H125(-0.0172)
;