Zero-valent metals in metal-organic frameworks: fac-M(CO)<sub>3</sub>(pyrazine)<sub>3/2</sub>.
Voigt, Laura; Wugt Larsen, René; Kubus, Mariusz; Pedersen, Kasper S.; Chemical communications (Cambridge, England) 57 (2021) 3861–3864; doi:10.1039/d1cc00864a

data_7128075
_publ_section_title
;
 Zero-valent metals in metal-organic frameworks:
 fac-M(CO)<sub>3</sub>(pyrazine)<sub>3/2</sub>.
;
_journal_issue                   32
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3861
_journal_page_last               3864
_journal_paper_doi               10.1039/d1cc00864a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C9 H6 Mo N3 O3, C2 H2 N'
_chemical_formula_sum            'C11 H8 Mo N4 O3'
_chemical_formula_weight         340.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-03-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-18 deposited with the CCDC.	2021-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                64.131(10)
_cell_angle_beta                 88.185(9)
_cell_angle_gamma                86.345(10)
_cell_formula_units_Z            2
_cell_length_a                   6.8571(8)
_cell_length_b                   9.7204(11)
_cell_length_c                   10.0406(10)
_cell_measurement_reflns_used    1262
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.0670
_cell_measurement_theta_min      4.7810
_cell_volume                     600.95(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3073
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     13.00  39.00   1.00  110.00    --   10.87 -99.00 120.00   26
  2  \w    -57.00  34.00   1.00  110.00    --   10.87 -57.00 120.00   91
  3  \w    -15.00  77.00   1.00  110.00    --   10.87  77.00  30.00   92
  4  \w    -16.00  83.00   1.00  110.00    --   10.87  57.00 -90.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0878018000
_diffrn_orient_matrix_UB_12      -0.0467549000
_diffrn_orient_matrix_UB_13      0.0211321000
_diffrn_orient_matrix_UB_21      0.0531043000
_diffrn_orient_matrix_UB_22      0.0655437000
_diffrn_orient_matrix_UB_23      -0.0151634000
_diffrn_orient_matrix_UB_31      -0.0146481000
_diffrn_orient_matrix_UB_32      -0.0107264000
_diffrn_orient_matrix_UB_33      0.0740777000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1047
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4212
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         3.679
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.101
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_description       needle
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         4212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0249P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3081
_reflns_number_total             4212
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9834\% 
 around [0.03 0.67 -0.75] (reciprocal) or [-0.00 0.71 -0.71] (direct)
;
_cod_data_source_file            d1cc00864a2.cif
_cod_data_source_block           lv194_moco3pyz2_e_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7128075--7128079.cif.'
_cod_database_code               7128075
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 H16 Mo2 N8 O8'
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.978
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6022(9)
 0.3978(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C7(H7), C9(H9), C11(H11)
;
_shelx_res_checksum              33986
_shelx_hkl_checksum              86493
_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 1.209
_oxdiff_exptl_absorpt_empirical_full_min 0.672
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2