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_7033847
_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
'C55 H99 Ca2 Mn6 O31, C45 H69 Mn3 N3 O13, 3(C2 H3 N)'
_chemical_formula_sum            'C106 H177 Ca2 Mn9 N6 O44'
_chemical_formula_weight         2814.14
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
'Moisture-sensitive, Hygroscopic, Efflorescent'
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2014-12-15 deposited with the CCDC.
2015-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.4452(4)
_cell_length_b                   24.4452(4)
_cell_length_c                   24.4452(4)
_cell_measurement_reflns_used    12858
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4578
_cell_measurement_theta_min      1.6661
_cell_volume                     14607.7(4)
_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, 2013)'
_computing_structure_solution
;
'XS (Sheldrick, 2013)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0146
_diffrn_orient_matrix_UB_12      0.0240
_diffrn_orient_matrix_UB_13      -0.0297
_diffrn_orient_matrix_UB_21      -0.0287
_diffrn_orient_matrix_UB_22      -0.0279
_diffrn_orient_matrix_UB_23      -0.0084
_diffrn_orient_matrix_UB_31      -0.0252
_diffrn_orient_matrix_UB_32      0.0178
_diffrn_orient_matrix_UB_33      0.0268
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.1079
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18874
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.457
_diffrn_reflns_theta_min         1.443
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             5888
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.208
_refine_ls_abs_structure_details
;
 Flack x determined using 2340 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.038(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         10502
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0892
_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^)+(0.1049P)^2^+15.7895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2094
_refine_ls_wR_factor_ref         0.2423
_reflns_Friedel_coverage         0.766
_reflns_Friedel_fraction_full    0.932
_reflns_Friedel_fraction_max     0.875
_reflns_number_gt                8138
_reflns_number_total             10502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03459g2.cif
_cod_data_source_block           ComplexC
_cod_depositor_comments
'Adding full bibliography for 7033847--7033849.cif.'
_cod_original_cell_volume        14607.7(7)
_cod_database_code               7033847
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.924
_diffrn_number_total             5963
_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
 O11B-C19 = O11-C19
 1.25 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O10B \\sim O10: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(O10) \\sim Ueq, Uanis(O10B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O11B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C28) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O10(0.33333) O10B(0.33333) O11(0.33333) O11B(0.33333)
5.a Aromatic/amide H refined with riding coordinates:
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
5.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              98437
_olex2_submission_special_instructions 'No special instructions were received'