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_7120016
_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 Mn5 N4 O17, 0.51(C4 H10 O), 0.49(C4 H8 O1), 2(C4 O)'
_chemical_formula_sum            'C128 H93.03 Mn5 N4 O20'
_chemical_formula_weight         2281.79
_chemical_name_systematic
;
 ?
;
_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             2017-03-08
_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                90.350(2)
_cell_angle_beta                 98.124(2)
_cell_angle_gamma                92.207(2)
_cell_formula_units_Z            2
_cell_length_a                   14.7524(8)
_cell_length_b                   16.2906(8)
_cell_length_c                   22.1991(12)
_cell_measurement_reflns_used    9147
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.363
_cell_measurement_theta_min      2.477
_cell_volume                     5277.2(5)
_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      100.04
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0384
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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            130593
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.156
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0540 before and 0.0455 after correction. The Ratio of minimum to maximum transmission is 0.9610. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       block
_exptl_crystal_F_000             2348
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.7465
_exptl_transmission_factor_min   0.7174
_refine_diff_density_max         1.689
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1412
_refine_ls_number_reflns         32156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+7.8870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1394
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24566
_reflns_number_total             32156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02313h2.cif
_cod_data_source_block           4
_cod_database_code               7120016
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C124)=Sof(H12D)=Sof(H12E)=Sof(C122)=Sof(H12F)=Sof(H12G)=Sof(C121)=
 Sof(H12H)=Sof(H12I)=Sof(O18)=Sof(C123)=Sof(H12J)=Sof(H12K)=1-FVAR(1)
 Sof(O17)=Sof(C118)=Sof(H11I)=Sof(H11J)=Sof(H11K)=Sof(C119)=Sof(H11L)=
 Sof(H11M)=Sof(C120)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C117)=Sof(H11N)=
 Sof(H11O)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C114(H11A,H11B), C113(H11C,H11D), C116(H11E,H11F), C115(H11G,H11H), C119(H11L,
 H11M), C117(H11N,H11O), C124(H12D,H12E), C122(H12F,H12G), C121(H12H,H12I),
 C123(H12J,H12K)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C9(H9), C15(H15), C39(H39), C108(H108), C3(H3), C42(H42),
 C25(H25), C47(H47), C6(H6), C35(H35), C95(H95), C40(H40), C112(H112), C5(H5),
 C23(H23), C41(H41), C45(H45), C16(H16), C18(H18), C63(H63), C22(H22),
 C102(H102), C99(H99), C44(H44), C89(H89), C98(H98), C17(H17), C76(H76),
 C27(H27), C92(H92), C96(H96), C24(H24), C46(H46), C97(H97), C32(H32), C56(H56),
  C104(H104), C105(H105), C4(H4), C109(H109), C34(H34), C77(H77), C50(H50),
 C110(H110), C111(H111), C90(H90), C103(H103), C30(H30), C69(H69), C86(H86),
 C79(H79), C91(H91), C78(H78), C33(H33), C82(H82), C28(H28), C66(H66), C64(H64),
  C57(H57), C84(H84), C60(H60), C71(H71), C70(H70), C85(H85), C58(H58),
 C72(H72), C73(H73), C83(H83), C29(H29), C53(H53), C51(H51), C65(H65), C59(H59),
  C52(H52)
3.c Idealised Me refined as rotating group:
 C118(H11I,H11J,H11K), C120(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'