CaMn4O2 model of the biological Oxygen Evolving Complex: Synthesis by cluster expansion on low symmetry ligand
Lee, Heui Beom; Tsui, Emily Y.; Agapie, Theodor; Chem. Commun.  (2017) –; doi:10.1039/C7CC02313H

data_7120015
_publ_section_title
;
 CaMn4O2 model of the biological Oxygen Evolving Complex: Synthesis by
 cluster expansion on low symmetry ligand
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02313H
_journal_year                    2017
_chemical_formula_moiety
'C116 H84 Ca Mn4 N4 O17, 2(C H2 Cl2), 0.5(C4 H8 O)'
_chemical_formula_sum            'C120 H92 Ca Cl4 Mn4 N4 O17.5'
_chemical_formula_weight         2271.61
_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     dual
_audit_creation_date             2017-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-27 deposited with the CCDC.
2017-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                88.2880(10)
_cell_angle_beta                 81.0900(10)
_cell_angle_gamma                87.5960(10)
_cell_formula_units_Z            2
_cell_length_a                   14.8017(4)
_cell_length_b                   16.3782(5)
_cell_length_c                   21.9258(6)
_cell_measurement_reflns_used    9512
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.19
_cell_measurement_theta_min      2.51
_cell_volume                     5245.1(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            161254
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.523
_diffrn_reflns_theta_min         2.204
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0670 before and 0.0526 after correction. The Ratio of minimum to maximum transmission is 0.9512. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       blade
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.7097
_refine_diff_density_max         2.223
_refine_diff_density_min         -1.841
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1362
_refine_ls_number_reflns         31911
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1157
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.189
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+15.6342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1886
_refine_ls_wR_factor_ref         0.2124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22245
_reflns_number_total             31911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02313h2.cif
_cod_data_source_block           5
_cod_original_formula_sum        'C120 H92 Ca Cl4 Mn4 N4 O17.50'
_cod_database_code               7120015
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Cl2-C117 = Cl1-C117 = Cl3-C117 = Cl4-C117
 1.7 with sigma of 0.0001
 O18-C120 = O18-C123
 1.54 with sigma of 0.0001
 C121-C120 = C122-C123
 1.57 with sigma of 0.0001
 C121-C122
 1.48 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
O18 \\sim C123 \\sim C120 \\sim H12A \\sim H12B \\sim C122 \\sim H12C \\sim
H12D \\sim C121 \\sim H12G \\sim H12H \\sim H12E \\sim H12F \\sim O18 \\sim
C123 \\sim O18 \\sim C120 \\sim C123 \\sim H12A \\sim C123 \\sim H12B \\sim
C123 \\sim C122 \\sim C120 \\sim H12C \\sim C120 \\sim H12D \\sim C121 \\sim
C120 \\sim C122 \\sim C121 \\sim C122 \\sim H12G \\sim C122 \\sim H12H \\sim
C121 \\sim H12E \\sim C121 \\sim H12F: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Others
 Sof(H11K)=Sof(H11L)=Sof(Cl3)=Sof(Cl1)=1-FVAR(1)
 Sof(H11I)=Sof(H11J)=Sof(Cl4)=Sof(Cl2)=FVAR(1)
 Sof(C118)=Sof(H11O)=Sof(H11P)=1-FVAR(2)
 Sof(C119)=Sof(H11M)=Sof(H11N)=FVAR(2)
 Fixed Sof: O18(0.5) C123(0.5) H12A(0.5) H12B(0.5) C120(0.5) H12C(0.5)
 H12D(0.5) C121(0.5) H12E(0.5) H12F(0.5) C122(0.5) H12G(0.5) H12H(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C115(H11A,H11B), C117(H11I,H11J), C117(H11K,H11L), C113(H11C,H11D), C116(H11E,
 H11F), C114(H11G,H11H), C119(H11M,H11N), C123(H12A,H12B), C120(H12C,H12D),
 C121(H12E,H12F), C122(H12G,H12H), C118(H11O,H11P)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C13(H13), C47(H47), C56(H56), C44(H44), C57(H57), C82(H82),
 C60(H60), C50(H50), C53(H53), C15(H15), C35(H35), C3(H3), C42(H42), C45(H45),
 C86(H86), C16(H16), C39(H39), C30(H30), C76(H76), C34(H34), C46(H46), C58(H58),
  C6(H6), C59(H59), C32(H32), C27(H27), C40(H40), C41(H41), C51(H51), C17(H17),
 C5(H5), C83(H83), C52(H52), C18(H18), C79(H79), C85(H85), C77(H77), C63(H63),
 C29(H29), C4(H4), C25(H25), C84(H84), C33(H33), C28(H28), C78(H78), C89(H89),
 C22(H22), C69(H69), C73(H73), C95(H95), C102(H102), C72(H72), C24(H24),
 C23(H23), C99(H99), C96(H96), C70(H70), C66(H66), C64(H64), C90(H90), C97(H97),
  C92(H92), C98(H98), C108(H108), C71(H71), C91(H91), C65(H65), C103(H103),
 C109(H109), C104(H104), C105(H105), C112(H112), C110(H110), C111(H111)
;
_olex2_submission_special_instructions 'No special instructions were received'