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_7120014
_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         'C60 H48 Fe4 N5 O13, C4 H10 O'
_chemical_formula_sum            'C64 H58 Fe4 N5 O14'
_chemical_formula_weight         1344.55
_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                75.523(4)
_cell_angle_beta                 75.229(3)
_cell_angle_gamma                65.876(3)
_cell_formula_units_Z            2
_cell_length_a                   13.7237(14)
_cell_length_b                   13.9138(13)
_cell_length_c                   17.8609(17)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.39
_cell_volume                     2968.4(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 0.999
_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  0.1863
_diffrn_reflns_av_unetI/netI     0.1232
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            105521
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.264
_diffrn_reflns_theta_min         2.391
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.030
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0876 before and 0.0659 after correction. The Ratio of minimum to maximum transmission is 0.9607. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       block
_exptl_crystal_F_000             1386
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.7168
_refine_diff_density_max         1.668
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         14691
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1521
_refine_ls_R_factor_gt           0.0744
_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^)+(0.0631P)^2^+9.4315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8670
_reflns_number_total             14691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02313h2.cif
_cod_data_source_block           2
_cod_database_code               7120014
_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
 O14-C63 = O14-C61
 1.4 with sigma of 0.001
 C63-C64 = C61-C62
 1.5 with sigma of 0.001
 C61-C63
 2.32 with sigma of 0.001
 C64-C62
 4.7 with sigma of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C63(H63A,H63B)
3.b Aromatic/amide H refined with riding coordinates:
 C47(H47), C11(H11), C40(H40), C39(H39), C30(H30), C15(H15), C60(H60), C9(H9),
 C16(H16), C18(H18), C13(H13), C27(H27), C46(H46), C32(H32), C44(H44), C42(H42),
  C29(H29), C59(H59), C34(H34), C22(H22), C56(H56), C28(H28), C17(H17),
 C35(H35), C57(H57), C45(H45), C24(H24), C25(H25), C41(H41), C33(H33), C58(H58),
  C3(H3), C23(H23), C4(H4), C6(H6), C5(H5)
3.c Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C49(H49A,H49B,
 H49C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C)
;
_olex2_submission_original_sample_id 2
_olex2_submission_special_instructions 'No special instructions were received'