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_7128079
_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 N3 O3 W'
_chemical_formula_sum            'C9 H6 N3 O3 W'
_chemical_formula_weight         388.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-01-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-02-15 deposited with the CCDC.	2021-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.482(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8974(7)
_cell_length_b                   9.9861(5)
_cell_length_c                   6.7067(3)
_cell_measurement_reflns_used    3812
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.7990
_cell_measurement_theta_min      4.5440
_cell_volume                     1198.61(9)
_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 0.997
_diffrn_measured_fraction_theta_max 0.991
_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    -14.00  82.00   1.00   20.00    --   10.87  38.00 150.00   96
  2  \w    -69.00  31.00   1.00   20.00    --   10.87 -19.00 -30.00  100
  3  \w      3.00  52.00   1.00   20.00    --   10.87 -99.00-120.00   49
  4  \w      3.00  30.00   1.00   20.00    --   10.87 -38.00-120.00   27
  5  \w    -20.00  28.00   1.00   20.00    --  -11.58 -99.00 -60.00   48
;
_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      0.0022860000
_diffrn_orient_matrix_UB_12      0.0643413000
_diffrn_orient_matrix_UB_13      -0.0444418000
_diffrn_orient_matrix_UB_21      0.0070011000
_diffrn_orient_matrix_UB_22      0.0288264000
_diffrn_orient_matrix_UB_23      0.0950104000
_diffrn_orient_matrix_UB_31      0.0389378000
_diffrn_orient_matrix_UB_32      -0.0090077000
_diffrn_orient_matrix_UB_33      -0.0135394000
_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  0.0384
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5042
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         3.781
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.632
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88662
_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 yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.150
_exptl_crystal_description       needle
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.287
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1392
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0215
_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^)+(0.0199P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0421
_refine_ls_wR_factor_ref         0.0422
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1385
_reflns_number_total             1392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00864a2.cif
_cod_data_source_block           lv_wco3pyz_aferrevacat150degrees_120k
_cod_depositor_comments
'Adding full bibliography for 7128075--7128079.cif.'
_cod_database_code               7128079
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'W C9 N3 H6 O3'
_shelx_estimated_absorpt_t_max   0.644
_shelx_estimated_absorpt_t_min   0.249
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N1-C4
 1.345 with sigma of 0.02
 N2-C8
 1.345 with sigma of 0.02
 N2-C10
 1.345 with sigma of 0.02
 N1-C3
 1.345 with sigma of 0.02
 C7-N2 \\sim N2-C9
 with sigma of 0.02
 C9-N2 \\sim N2-C7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N2 \\sim C8 \\sim C10: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
N2 \\sim C7 \\sim C9: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3A) \\sim Ueq, Uanis(C4A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4A) \\sim Ueq, Uanis(C3A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 Sof(C4A)=Sof(H4A)=Sof(C3A)=Sof(H3A)=1-FVAR(1)
 Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=FVAR(1)
 Fixed Sof: C7(0.16667) H7(0.16667) C8(0.33333) C9(0.16667) H9(0.16667)
 C10(0.33333) H8(0.33333) H10(0.33333)
 Fixed Uiso: H8(0.024) H10(0.024)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C9(H9), C4A(H4A), C3A(H3A)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 78 electrons were 
found in a volume of 216 A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.25[C4H4N2] per Asymmetric Unit 
which account for 84 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              92889
_shelx_hkl_checksum              42669
_shelx_fab_checksum              8956
_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 1.152
_oxdiff_exptl_absorpt_empirical_full_min 0.906