Photoactive carbon monoxide-releasing coordination polymer particles
Carné-Sánchez, Arnau; Ikemura, Shuya; Sakaguchi, Reiko; Craig, Gavin A.; Furukawa, Shuhei; Chemical Communications  (2022) –; doi:10.1039/D2CC03907A

data_7130555
_publ_section_title
;
 Photoactive carbon monoxide-releasing coordination polymer particles
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03907A
_journal_year                    2022
_chemical_formula_moiety         'Br, C33 H30 Mn N6 O3'
_chemical_formula_sum            'C33 H30 Br Mn N6 O3'
_chemical_formula_weight         693.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-28 deposited with the CCDC.	2022-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.478(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.0896(6)
_cell_length_b                   9.7834(2)
_cell_length_c                   20.0973(3)
_cell_measurement_reflns_used    23708
_cell_measurement_temperature    93
_cell_measurement_theta_max      29.1560
_cell_measurement_theta_min      2.1400
_cell_volume                     6269.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     37.00  66.00   0.50    8.00    --  -23.00  45.00 160.96   58
  2  \w   -111.00 -84.00   0.50    8.00    --  -23.00  45.00  60.00   54
  3  \w    -74.00 -48.00   0.50    8.00    --  -23.00  45.00  60.00   52
  4  \w    -36.00   3.00   0.50    8.00    --  -23.00  45.00  60.00   78
  5  \w     21.00  66.00   0.50    8.00    --  -23.00  45.00  60.00   90
  6  \w   -106.00  66.00   0.50    8.00    --  -23.00  45.00   0.00  344
  7  \w   -112.00 -18.00   0.50    8.00    --  -23.00  45.00 120.00  188
  8  \w     39.00  66.00   0.50    8.00    --  -23.00  45.00 120.00   54
  9  \w    -73.00  65.00   0.50    8.00    --  -23.00  45.00  30.00  276
 10  \w   -112.00 -87.00   0.50    8.00    --  -23.00  45.00 150.00   50
 11  \w    -57.00 -32.00   0.50    8.00    --  -23.00  45.00 150.00   50
 12  \w     -6.00  47.00   0.50    8.00    --  -23.00  45.00 150.00  106
 13  \w    -32.00  -7.00   0.50    8.00    --  -23.00  45.00  90.00   50
 14  \w     20.00  65.00   0.50    8.00    --  -23.00  45.00  90.00   90
 15  \w   -112.00 -41.00   0.50    8.00    --  -23.00  45.00 160.96  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0186869000
_diffrn_orient_matrix_UB_12      0.0185763000
_diffrn_orient_matrix_UB_13      0.0135696000
_diffrn_orient_matrix_UB_21      0.0113730000
_diffrn_orient_matrix_UB_22      0.0054035000
_diffrn_orient_matrix_UB_23      0.0322566000
_diffrn_orient_matrix_UB_31      0.0040496000
_diffrn_orient_matrix_UB_32      0.0698555000
_diffrn_orient_matrix_UB_33      -0.0060816000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42157
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.237
_diffrn_reflns_theta_min         2.040
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.740
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.506
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.103(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         13888
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0991P)^2^+11.7270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1384
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    0.814
_reflns_Friedel_fraction_max     0.687
_reflns_number_gt                12800
_reflns_number_total             13888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03907a2.cif
_cod_data_source_block           si146_model_bim
_cod_database_code               7130555
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         MnBrC33H30N6O3
_shelx_estimated_absorpt_t_max   0.845
_shelx_estimated_absorpt_t_min   0.623
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.897(9)
 0.103(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C54(H54A,H54B), C44(H44A,H44B), C14(H14A,H14B), C4(H4A,H4B),
 C24(H24A,H24B)
3.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C56(H56), C42(H42), C7(H7), C33(H33), C41(H41), C43(H43), C10(H10),
 C6(H6), C23(H23), C53(H53), C1(H1), C22(H22), C21(H21), C28(H28), C11(H11),
 C40(H40), C27(H27), C59(H59), C60(H60), C9(H9), C8(H8), C58(H58), C52(H52),
 C20(H20), C57(H57), C16(H16), C17(H17), C50(H50), C36(H36), C31(H31), C32(H32),
  C38(H38), C12(H12), C29(H29), C3(H3), C26(H26), C39(H39), C13(H13), C30(H30),
 C46(H46), C19(H19), C37(H37), C48(H48), C47(H47), C49(H49), C2(H2), C18(H18)
;
_shelx_res_checksum              98237
_shelx_hkl_checksum              52508
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.690
_oxdiff_exptl_absorpt_empirical_full_min 0.608