Studying manganese carbonyl photochemistry in a permanently porous metal-organic framework.
Young, Rosemary J.; Huxley, Michael T.; Wu, Lingjun; Hart, Jack; O'Shea, James; Doonan, Christian J.; Champness, Neil R.; Sumby, Christopher J.; Chemical science 14 (2023) 9409–9417; doi:10.1039/d3sc03553k

data_1569675
_publ_section_title
;
 Studying manganese carbonyl photochemistry in a permanently porous
 metal-organic framework.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              9409
_journal_page_last               9417
_journal_paper_doi               10.1039/d3sc03553k
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety
'C39.55 H35.8 Br0.25 Mn1.85 N6 O7, 0.1(Br), C4 H8 O'
_chemical_formula_sum            'C43.5 H43.8 Br0.35 Mn1.85 N6 O7.95'
_chemical_formula_weight         907.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2022-10-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-11-11 deposited with the CCDC.	2023-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.93(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.344(3)
_cell_length_b                   32.785(7)
_cell_length_c                   12.996(3)
_cell_measurement_reflns_used    88484
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.684
_cell_measurement_theta_min      1.242
_cell_volume                     5247(2)
_computing_cell_refinement       'AS QEGUI'
_computing_data_collection       'XDS (Kabsch, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean '13.3 (Dectris Eiger detectors)'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.800
_diffrn_measurement_device_type
;
N. P. Cowieson, D. Aragao, M. Clift, D. J. Ericsson, C. Gee, 
S. J. Harrop, N. Mudie, S. Panjikar, J. R. Price, A. Riboldi-
Tunnicliffe, R. Williamson and T. Caradoc-Davies, MX1: a 
bending-magnet crystallography beamline serving both chemical 
and macromolecular crystallography communities at the 
Australian Synchrotron, J. Synchrotron Rad. (2015). 22, 187-190.
;
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.800
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            88484
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.800
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         31.684
_diffrn_reflns_theta_min         1.242
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       plate
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.105
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         14436
_refine_ls_number_restraints     263
_refine_ls_restrained_S_all      1.293
_refine_ls_R_factor_all          0.1506
_refine_ls_R_factor_gt           0.1136
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3302
_refine_ls_wR_factor_ref         0.3554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8939
_reflns_number_total             14436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03553k2.cif
_cod_data_source_block           mnbr_e1_thf_30m270k
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1569673--1569679.cif.
;
_cod_original_cell_volume        5247.1(18)
_cod_original_formula_sum        'C43.50 H43.80 Br0.35 Mn1.85 N6 O7.95'
_cod_database_code               1569675
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.875
_diffrn_measurement_detector_type 'Dectris Eiger2 9M'
_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, All C(H,H,H,H,H,H,H,H) groups
2. Restrained distances
 Mn3-C110
 1.84 with sigma of 0.02
 C110-O111
 1.12 with sigma of 0.02
 Mn3-C112
 1.84 with sigma of 0.02
 Mn3-Br2
 2.6 with sigma of 0.02
 C112-O113
 1.12 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C110 \\sim O111: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O2 \\sim C3 \\sim C7 \\sim C8 \\sim C9: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
O1 \\sim C2 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C112 \\sim O113: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C110) \\sim Ueq, Uanis(O111) \\sim Ueq, Uanis(C112) \\sim Ueq,
Uanis(O113) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim
Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 C110, O111
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C71, C72, C73, C74, C75, C76
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C3, C7, C8, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C2, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C112, O113
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C23B)=Sof(H23B)=Sof(C25B)=Sof(H25B)=Sof(C22B)=Sof(H22B)=Sof(C26B)=
 Sof(H26B)=1-FVAR(1)
 Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=FVAR(1)
 Fixed Sof: Br1(0.2) Br3(0.1) Mn3(0.35) C110(0.3) O111(0.3) C112(0.35)
 O113(0.35) Br2(0.05) O1(0.35) C2(0.35) C4(0.35) C5(0.35) C6(0.35) H2(0.35)
 H1(0.35) H4A(0.35) H4B(0.35) H5A(0.35) H5B(0.35) H6A(0.35) H6B(0.35)
6.a Free rotating group:
 O2(C3,C7,C8,C9,H3A,H3B,H7A,H7B,H8A,H8B,H9A,H9B), O1(C2,C4,C5,C6,H2,H1,H4A,H4B,
 H5A,H5B,H6A,H6B)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C50(H50A,H50B)
6.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C25(H25), C26(H26), C42(H42), C43(H43), C45(H45),
 C46(H46), C72(H72), C73(H73), C75(H75), C76(H76), C23B(H23B), C25B(H25B),
 C22B(H22B), C26B(H26B)
6.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 310 electrons were 
found in a volume of 1158\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C4H8O] per Asymmetric Unit 
which account for 320 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              17662
_shelx_fab_checksum              97121
_olex2_submission_special_instructions 'No special instructions were received'