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_7120017
_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
'C99 H67 Mn4 N4 O13, 1.28(C H2 Cl2), 0.65(C4 H10 O)'
_chemical_formula_sum            'C102.89 H76.08 Cl2.56 Mn4 N4 O13.65'
_chemical_formula_weight         1897.34
_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                77.057(3)
_cell_angle_beta                 82.240(3)
_cell_angle_gamma                83.778(3)
_cell_formula_units_Z            2
_cell_length_a                   13.5028(18)
_cell_length_b                   16.598(2)
_cell_length_c                   21.517(3)
_cell_measurement_reflns_used    9319
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.912
_cell_measurement_theta_min      2.320
_cell_volume                     4641.5(11)
_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      99.99
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            132477
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.747
_diffrn_reflns_theta_min         1.901
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0671 before and 0.0582 after correction. The Ratio of minimum to maximum transmission is 0.8906. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       block
_exptl_crystal_F_000             1948
_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   0.6645
_refine_diff_density_max         2.220
_refine_diff_density_min         -1.476
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         28763
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0902
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0990P)^2^+25.4332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2506
_refine_ls_wR_factor_ref         0.2746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18769
_reflns_number_total             28763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02313h2.cif
_cod_data_source_block           1
_cod_original_cell_volume        4641.4(11)
_cod_database_code               7120017
_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. Restrained distances
 Cl4-C105 = Cl3-C105
 1.7 with sigma of 0.001
 Cl3-Cl4
 2.88 with sigma of 0.001
 Cl6-C106 = Cl5-C106
 1.7 with sigma of 0.001
 Cl5-C106 = Cl6-C106
 1.7 with sigma of 0.0001
 Cl6-Cl5
 2.9 with sigma of 0.0001
3. Others
 Sof(O14)=Sof(C101)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C102)=Sof(H10D)=
 Sof(H10E)=Sof(C103)=Sof(H10F)=Sof(H10G)=Sof(C104)=Sof(H10H)=Sof(H10I)=
 Sof(H10J)=FVAR(1)
 Sof(Cl3)=Sof(Cl4)=Sof(C105)=Sof(H10M)=Sof(H10N)=FVAR(2)
 Fixed Sof: Cl5(0.2) Cl6(0.2) C106(0.2) H10O(0.2) H10P(0.2)
4.a Secondary CH2 refined with riding coordinates:
 C100(H10K,H10L), C105(H10M,H10N), C106(H10O,H10P), C102(H10D,H10E), C103(H10F,
 H10G)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27),
  C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35),
 C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
  C50(H50), C51(H51), C52(H52), C53(H53), C56(H56), C57(H57), C58(H58),
 C59(H59), C60(H60), C63(H63), C64(H64), C65(H65), C66(H66), C69(H69), C70(H70),
  C71(H71), C72(H72), C73(H73), C76(H76), C77(H77), C78(H78), C79(H79),
 C82(H82), C83(H83), C84(H84), C85(H85), C86(H86), C89(H89), C90(H90), C91(H91),
  C92(H92), C99(H99), C98(H98), C97(H97), C96(H96), C95(H95)
4.c Fitted hexagon refined as free rotating group:
 C55(C56,C57,C58,C59,C60), C68(C69,C70,C71,C72,C73), C81(C82,C83,C84,C85,C86),
 C94(C99,C98,C97,C96,C95)
4.d Idealised Me refined as rotating group:
 C101(H10A,H10B,H10C), C104(H10H,H10I,H10J)
;
_olex2_submission_special_instructions 'No special instructions were received'