Artificial synthetic Mn(IV)Ca-oxido complexes mimic the oxygen-evolving complex in photosystem II.
Chen, Changhui; Zhang, Chunxi; Dong, Hongxing; Zhao, Jingquan; Dalton transactions (Cambridge, England : 2003) 44 (2015) 4431–4435; doi:10.1039/c4dt03459g

data_7033849
_publ_section_title
;
 Artificial synthetic Mn(IV)Ca-oxido complexes mimic the oxygen-evolving
 complex in photosystem II.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4431
_journal_page_last               4435
_journal_paper_doi               10.1039/c4dt03459g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'C54 H104 Ca2 Mn6 O34, 3(C5 H10 O2), C4 H8 O2'
_chemical_formula_sum            'C73 H142 Ca2 Mn6 O42'
_chemical_formula_weight         2101.66
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
'Moisture-sensitive, Hygroscopic, Efflorescent'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2014-12-15 deposited with the CCDC.
2015-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.39(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.486(5)
_cell_length_b                   30.822(6)
_cell_length_c                   26.925(4)
_cell_measurement_reflns_used    32531
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4801
_cell_measurement_theta_min      1.3213
_cell_volume                     20734(7)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
'XS (Sheldrick, 2008)' 
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0105
_diffrn_orient_matrix_UB_12      -0.0209
_diffrn_orient_matrix_UB_13      -0.0317
_diffrn_orient_matrix_UB_21      -0.0108
_diffrn_orient_matrix_UB_22      -0.0238
_diffrn_orient_matrix_UB_23      0.0193
_diffrn_orient_matrix_UB_31      -0.0411
_diffrn_orient_matrix_UB_32      0.0022
_diffrn_orient_matrix_UB_33      -0.0203
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0862
_diffrn_reflns_av_unetI/netI     0.0880
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            70319
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         1.039
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.50483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             8848
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: C2H5O2CCH3'
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.203
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1183
_refine_ls_number_reflns         23662
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      1.277
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.1067
_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^)+(0.0246P)^2^+123.6285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1816
_refine_ls_wR_factor_ref         0.1914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19570
_reflns_number_total             23662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03459g2.cif
_cod_data_source_block           ComplexB
_cod_depositor_comments
'Adding full bibliography for 7033847--7033849.cif.'
_cod_database_code               7033849
_shelxl_version_number           2013-4
_diffrn_number_total             24124
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C63-C62
 1.54 with sigma of 0.01
 C29-C28 = C29-C27 = C29-C27A = C29-C26 = C29-C26A = C29-C28A
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C27A \\sim C28A \\sim C26A: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
C28 \\sim C29 \\sim C26 \\sim C60 \\sim O37 \\sim C61 \\sim O38 \\sim C62 \\sim
C63 \\sim C51 \\sim C52 \\sim O31 \\sim C53 \\sim C54 \\sim C48 \\sim C46 \\sim
C47 \\sim C49 \\sim C64 \\sim C65 \\sim C66 \\sim C70 \\sim C71 \\sim C69:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C27A) \\sim Ueq, Uanis(C28A) \\sim Ueq, Uanis(C26A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(O37) \\sim Ueq, Uanis(O38)
\\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C70) \\sim Ueq,
Uanis(C71) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq,
Uanis(O31) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C48) \\sim Ueq,
Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
: with sigma of 0.005 and sigma for terminal atoms of 0.02
4. Others
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
5.a Rotating group:
 O32(H32A,H32B), O33(H33A,H33B), O34(H34A,H34B)
5.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C62(H62A,H62B)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,
 H13B,H13C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C32(H32C,
 H32D,H32E), C33(H33C,H33D,H33E), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C51(H51A,
 H51B,H51C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C),
 C57(H57A,H57B,H57C), C60(H60A,H60B,H60C), C63(H63A,H63B,H63C), C26A(H26D,H26E,
 H26F), C27A(H27D,H27E,H27F), C28A(H28D,H28E,H28F), C64(H64A,H64B,H64C),
 C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C69(H69A,H69B,H69C), C70(H70A,H70B,
 H70C), C71(H71A,H71B,H71C)
5.d Idealised tetrahedral OH refined as rotating group:
 O35(H35), O40(H40), O41(H41)
;
_shelx_res_checksum              48511