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_1569677
_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
'C40.3 H38.6 Br0.275 Mn1.85 N6 O6.7, C4 H8 O, 0.075(Br)'
_chemical_formula_sum            'C44.3 H43.6 Br0.35 Mn1.85 N6 O7.7'
_chemical_formula_weight         912.86
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-10-31
_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                 93.82(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.338(3)
_cell_length_b                   32.702(7)
_cell_length_c                   13.010(3)
_cell_measurement_reflns_used    78054
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      1.245
_cell_volume                     5238(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      100(2)
_diffrn_detector_area_resol_mean '13.3 (Dectris Eiger detectors)'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0546
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            78054
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.245
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       plate
_exptl_crystal_F_000             1886
_exptl_crystal_preparation       'Photolysis led to lightening of the crystal'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.522
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.404
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         12158
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      1.414
_refine_ls_R_factor_all          0.1378
_refine_ls_R_factor_gt           0.1121
_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          0.3294
_refine_ls_wR_factor_ref         0.3533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8555
_reflns_number_total             12158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03553k2.cif
_cod_data_source_block           e190
_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        5237.6(18)
_cod_original_formula_sum        'C44.30 H43.60 Br0.35 Mn1.85 N6 O7.70'
_cod_database_code               1569677
_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
2. Restrained distances
 Br2-Mn3
 2.6 with sigma of 0.02
 Br1-Mn3B
 2.65 with sigma of 0.02
 Mn3-N61
 -2.2 with sigma of 0.02
 C63-C66
 1.5 with sigma of 0.02
 C65-C67
 1.5 with sigma of 0.02
 N61-N62
 1.35 with sigma of 0.02
3. Restrained planarity
 C71, C72, C73, C74, C75, C76
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O81 \\sim C82 \\sim C83 \\sim C84 \\sim C85: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
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
O2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 O81, C82, C83, C84, C85
 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, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{O81, C82, C83, C84, C85} sigma for 1-2: 0.02, 1-3: 0.04
as in
{Br10, Mn3B, O2, C3, C4}
7. Others
 Fixed Sof: Br1(0.165) Br2(0.11) Mn3(0.175) Br10(0.075) Mn3B(0.175) O2(0.7)
 C3(0.7) H3A(0.7) H3B(0.7) C4(0.7) H4A(0.7) H4B(0.7) C5(0.7) H5A(0.7) H5B(0.7)
 C6(0.7) H6A(0.7) H6B(0.7)
8.a Free rotating group:
 O2(C3,C4,C5,C6)
8.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C51(H51A,H51B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B),
 C85(H85A,H85B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
8.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)
8.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 280 electrons were 
found in a volume of 1134\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.875[C4H8O] per Asymmetric Unit 
which account for 280 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              58620
_shelx_fab_checksum              59456
_olex2_submission_special_instructions 'No special instructions were received'