Hybrid bronzes: mixed-valence organic-inorganic metal oxides as a tunable material platform.
Dayaratne, W Lakna N; Torres-Cadena, Raúl; Schmitt, Bennett P.; Westrick, Emma M.; Jaffe, Adam; Chemical science 14 (2023) 10756–10767; doi:10.1039/d3sc03828a

data_1569870
_publ_section_title
;
 Hybrid bronzes: mixed-valence organic-inorganic metal oxides as a tunable
 material platform.
;
_journal_issue                   39
_journal_name_full               'Chemical science'
_journal_page_first              10756
_journal_page_last               10767
_journal_paper_doi               10.1039/d3sc03828a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C5 H4 Mo N2 O3'
_chemical_formula_sum            'C5 H4 Mo N2 O3'
_chemical_formula_weight         236.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-07-14
_audit_creation_method
;FinalCif V123 by Daniel Kratzert, Freiburg 2023, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2023-07-18 deposited with the CCDC.	2023-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.522(3)
_cell_length_b                   7.375(3)
_cell_length_c                   25.795(11)
_cell_measurement_reflns_used    3004
_cell_measurement_temperature    120.01
_cell_measurement_theta_max      26.360
_cell_measurement_theta_min      3.159
_cell_volume                     1431.0(10)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2021)'
_computing_data_collection       'Bruker APEX-4 (Bruker, 2021)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2021)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2020)'
_computing_publication_material
'FinalCIF (Kratzert, 2023)/CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      120.01
_diffrn_detector                 'CCD Area Detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker APEX-II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       'combination of \w and \f-scans'
_diffrn_radiation_monochromator  'Bruker TRIUMPH curved-graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            15450
_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         26.017
_diffrn_reflns_theta_min         1.579
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.787
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_correction_T_min  0.8076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0670 before and 0.0569 after correction.
The Ratio of minimum to maximum transmission is 0.8427.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.191
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_recrystallization_method
'Hydrothermal reaction at 95C for 24 h followed by 80C for 3 days'
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.021
_refine_diff_density_max         4.363
_refine_diff_density_min         -4.043
_refine_diff_density_rms         0.318
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1402
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0814
_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^)+(0.0001P)^2^+102.6131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1693
_refine_ls_wR_factor_ref         0.1753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1160
_reflns_number_total             1402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03828a2.cif
_cod_data_source_block           aj1-azp0p5MoO3
_cod_depositor_comments
'Adding full bibliography for 1569868--1569870.cif.'
_cod_database_code               1569870
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Mo1 \\sim O3: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O1 \\sim Mo1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C6(H6), C5(H5)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.963
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 700'
_shelx_res_checksum              69512