Structurally characterized terminal manganese(iv) oxo tris(alkoxide) complex.
Halbach, Robert L.; Gygi, David; Bloch, Eric D.; Anderson, Bryce L.; Nocera, Daniel G.; Chemical science 9 (2018) 4524–4528; doi:10.1039/c8sc01164h

data_1549310
_publ_section_title
;
 Structurally characterized terminal manganese(iv) oxo tris(alkoxide)
 complex.
;
_journal_issue                   19
_journal_name_full               'Chemical science'
_journal_page_first              4524
_journal_page_last               4528
_journal_paper_doi               10.1039/c8sc01164h
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C30 H63 Mn O4, C20 H40 K O10'
_chemical_formula_sum            'C50 H103 K Mn O14'
_chemical_formula_weight         1022.36
_chemical_properties_physical    Moisture-sensitive
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-12 deposited with the CCDC.
2018-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                81.9430(10)
_cell_angle_beta                 88.4630(10)
_cell_angle_gamma                69.6350(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5253(8)
_cell_length_b                   16.1662(11)
_cell_length_c                   16.7311(12)
_cell_measurement_reflns_used    3848
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.049
_cell_measurement_theta_min      2.276
_cell_volume                     2892.8(4)
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_reduction        'SAINT V8.32B (?, 2016)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.98
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0861
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28035
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.230
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.357
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0823 before and 0.0550 after correction.
The Ratio of minimum to maximum transmission is 0.6169.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.327
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         11657
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0426P)^2^+0.0798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7597
_reflns_number_total             11657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01164h2.cif
_cod_data_source_block           cmpd_3_mn(o)(ditox)3k(15c5)2
_cod_depositor_comments
'Adding full bibliography for 1549310--1549312.cif.'
_cod_original_cell_volume        2892.8(3)
_cod_database_code               1549310
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.887
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 O5A, C31A, C32A, O6A, C33A, C34A, O7A, C35A, C36A, O8A, C37A, C38A, O9A, C39A,
  C40A, O5B, C31B, C32B, O6B, C33B, C34B, O7B, C35B, C36B, O8B, C37B, C38B, O9B,
  C39B, C40B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(O5B)=Sof(C31B)=Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=Sof(O6B)=
 Sof(C33B)=Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34C)=Sof(H34D)=Sof(O7B)=Sof(C35B)=
 Sof(H35C)=Sof(H35D)=Sof(C36B)=Sof(H36C)=Sof(H36D)=Sof(O8B)=Sof(C37B)=Sof(H37C)=
 Sof(H37D)=Sof(C38B)=Sof(H38C)=Sof(H38D)=Sof(O9B)=Sof(C39B)=Sof(H39C)=Sof(H39D)=
 Sof(C40B)=Sof(H40C)=Sof(H40D)=1-FVAR(1)
 Sof(O5A)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(O6A)=
 Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(O7A)=Sof(C35A)=
 Sof(H35A)=Sof(H35B)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(O8A)=Sof(C37A)=Sof(H37A)=
 Sof(H37B)=Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(O9A)=Sof(C39A)=Sof(H39A)=Sof(H39B)=
 Sof(C40A)=Sof(H40A)=Sof(H40B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C31A(H31A,H31B), C32A(H32A,H32B), C33A(H33A,H33B), C34A(H34A,H34B), C35A(H35A,
 H35B), C36A(H36A,H36B), C37A(H37A,H37B), C38A(H38A,H38B), C39A(H39A,H39B),
 C40A(H40A,H40B), C31B(H31C,H31D), C32B(H32C,H32D), C33B(H33C,H33D), C34B(H34C,
 H34D), C35B(H35C,H35D), C36B(H36C,H36D), C37B(H37C,H37D), C38B(H38C,H38D),
 C39B(H39C,H39D), C40B(H40C,H40D), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,
 H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
 C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B)
4.b Idealised Me refined as rotating group:
 C3(H,HA,HB), C4(HC,HD,HE), C5(HF,HG,HH), C6(HI,HJ,HK), C8(HL,HM,HN), C9(HO,HP,
 HQ), C10(HR,HS,HT), C13(HU,HV,HW), C14(HX,HY,HZ), C15(H0AA,H1AA,H2AA),
 C17(H3AA,H4AA,H5AA), C18(H6AA,H7AA,H8AA), C19(H9AA,H0BA,H1BA), C20(H2BA,H3BA,
 H4BA), C23(H5BA,H6BA,H7BA), C24(H8BA,H9BA,H0CA), C25(H1CA,H2CA,H3CA), C27(H4CA,
 H5CA,H6CA), C28(H7CA,H8CA,H9CA), C29(H0DA,H1DA,H2DA), C30(H3DA,H4DA,H5DA)
;
_shelx_res_checksum              75978
_olex2_submission_special_instructions 'No special instructions were received'