An organic-organometallic CO-releasing material comprising 4,4'-bipyridine and molybdenum subcarbonyl building blocks.
Calhau, Isabel B.; Gomes, Ana C.; Mendes, Ricardo F.; Almeida Paz, Filipe A.; Gonçalves, Isabel S; Pillinger, Martyn; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12783–12796; doi:10.1039/d4dt01303d

data_7716683
_publ_section_title
;
 An organic-organometallic CO-releasing material comprising
 4,4'-bipyridine and molybdenum subcarbonyl building blocks.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12783
_journal_page_last               12796
_journal_paper_doi               10.1039/d4dt01303d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C45 H40 Mo N4 O4'
_chemical_formula_weight         796.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-06-11 deposited with the CCDC.	2024-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.202(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.7557(3)
_cell_length_b                   10.6519(2)
_cell_length_c                   11.7860(3)
_cell_measurement_reflns_used    9240
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      26.1330
_cell_measurement_theta_min      2.2950
_cell_volume                     1974.93(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.949
_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     41.00  73.00   0.50   30.00    --    9.34   3.00  88.00   64
  2  \w    -59.00 -33.00   0.50   30.00    --    9.34   3.00  88.00   52
  3  \w    -28.00  -3.00   0.50   30.00    --    9.34  -3.00 -89.00   50
  4  \w     15.00  66.00   0.50   30.00    --  -10.12   3.00  88.00  102
  5  \w     -6.00  73.00   0.50   30.00    --    9.34  38.00 -30.00  158
  6  \w     14.00  57.00   0.50   30.00    --    9.34-125.00-180.00   86
  7  \w     -7.00  72.00   0.50   30.00    --    9.34  19.00-120.00  158
  8  \w    -48.00 -17.00   0.50   30.00    --  -10.12 125.00 120.00   62
  9  \w    -58.00 -30.00   0.50   30.00    --  -10.12 125.00  60.00   56
 10  \w    -44.00 -12.00   0.50   30.00    --  -10.12 125.00 -30.00   64
 11  \w    -24.00  49.00   0.50   30.00    --  -10.12  38.00 -90.00  146
 12  \w    -52.00 -27.00   0.50   30.00    --  -10.12 -38.00 120.00   50
 13  \w    -23.00   2.00   0.50   30.00    --  -10.12 -99.00-180.00   50
 14  \w    -14.00  21.00   0.50   30.00    --  -10.12 -99.00-120.00   70
 15  \w    -50.00 -23.00   0.50   30.00    --  -10.12 125.00  30.00   54
 16  \w    -10.00  16.00   0.50   30.00    --  -10.12 -99.00  30.00   52
 17  \w    -10.00  15.00   0.50   30.00    --  -10.12  -3.00 -89.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0023478000
_diffrn_orient_matrix_UB_12      0.0031569000
_diffrn_orient_matrix_UB_13      -0.0598617000
_diffrn_orient_matrix_UB_21      0.0450169000
_diffrn_orient_matrix_UB_22      -0.0002215000
_diffrn_orient_matrix_UB_23      0.0064699000
_diffrn_orient_matrix_UB_31      -0.0000647000
_diffrn_orient_matrix_UB_32      -0.0665099000
_diffrn_orient_matrix_UB_33      -0.0031245000
_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  0.0245
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10468
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.258
_diffrn_reflns_theta_min         2.309
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       plate
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.508
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 1433 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.344(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3484
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.136
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.2726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.737
_reflns_Friedel_fraction_full    0.854
_reflns_Friedel_fraction_max     0.783
_reflns_number_gt                3427
_reflns_number_total             3484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01303d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7716683--7716684.cif.'
_cod_original_cell_volume        1974.92(8)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7716683
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.830
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              22015
_shelx_hkl_checksum              19138