Iron polypyridyl complex adsorbed on carbon surfaces for hydrogen generation.
Margonis, Caroline M.; Ho, Marissa; Travis, Benjamin D.; Brennessel, William W.; McNamara, William R.; Chemical communications (Cambridge, England) 57 (2021) 7697–7700; doi:10.1039/d1cc02131a

data_7128585
_publ_section_title
;
 Iron polypyridyl complex adsorbed on carbon surfaces for hydrogen
 generation.
;
_journal_issue                   62
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7697
_journal_page_last               7700
_journal_paper_doi               10.1039/d1cc02131a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C30 H25 Cl2 Fe N4 O2'
_chemical_formula_sum            'C30 H25 Cl2 Fe N4 O2'
_chemical_formula_weight         600.29
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-09-30
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2021-04-16 deposited with the CCDC.	2021-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4056(2)
_cell_length_b                   22.8180(4)
_cell_length_c                   25.3841(5)
_cell_measurement_reflns_used    13400
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      73.1600
_cell_measurement_theta_min      3.5210
_cell_volume                     6606.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_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    -50.00  22.00   0.50    5.51    --  -49.62  51.00-127.00  144
  2  \w     -3.00  24.00   0.50    5.51    --  -49.62  19.00 -30.00   54
  3  \w     32.00 122.00   0.50    5.51    --   49.62  70.00  57.00  180
  4  \w     88.00 163.00   0.50   22.86    --  105.75  70.00  57.00  150
  5  \w    153.00 178.00   0.50   22.86    --  105.75  30.00 120.00   50
  6  \w     95.00 154.00   0.50   22.86    --  105.75 125.00  90.00  118
  7  \w     99.00 129.00   0.50   22.86    --  105.75  30.00 120.00   60
  8  \w     95.00 178.00   0.50   22.86    --  105.75 121.00 -62.00  166
  9  \w     40.00  65.00   0.50   22.86    --  105.75 -51.00  85.00   50
 10  \w     35.00  78.00   0.50   22.86    --  105.75 -61.00 -30.00   86
 11  \w     56.00  99.00   0.50   22.86    --  105.75 -94.00 -60.00   86
 12  \w     38.00  83.00   0.50   22.86    --  105.75 -61.00-120.00   90
 13  \w     52.00 109.00   0.50   22.86    --  105.75-125.00-180.00  114
 14  \w     36.00  83.00   0.50   22.86    --  105.75 -61.00-150.00   94
 15  \w     -9.00  17.00   0.50    5.51    --   49.62 -19.00-180.00   52
 16  \w   -120.00 -77.00   0.50    5.51    --  -49.62-121.00-144.00   86
 17  \w   -156.00 -73.00   0.50   22.86    --  -84.25-121.00-144.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0299209000
_diffrn_orient_matrix_UB_12      -0.0392781000
_diffrn_orient_matrix_UB_13      -0.0475048000
_diffrn_orient_matrix_UB_21      0.1310063000
_diffrn_orient_matrix_UB_22      0.0146487000
_diffrn_orient_matrix_UB_23      0.0068760000
_diffrn_orient_matrix_UB_31      0.0139366000
_diffrn_orient_matrix_UB_32      -0.0529320000
_diffrn_orient_matrix_UB_33      0.0371077000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41178
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         78.003
_diffrn_reflns_theta_min         3.482
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.388
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       plate
_exptl_crystal_F_000             2472
_exptl_crystal_recrystallization_method 'Solvent-solvent diffusion'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         6941
_refine_ls_number_restraints     250
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0923P)^2^+3.3164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5181
_reflns_number_total             6941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02131a2.cif
_cod_data_source_block           cwmwm15
_cod_depositor_comments          'Adding full bibliography for 7128585.cif.'
_cod_database_code               7128585
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.428
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C20-C22 \\sim C20-C22'
 with sigma of 0.01
3. Restrained planarity
 C20, C21', C22', C23', C24', C25', C26', C27', C28', C29', C30'
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.2A
5. Rigid body (RIGU) restrains
 C21, C22, C23, C24, C25, C26, C27, C28, C29, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21', C22', C23', C24', C25', C26', C27', C28', C29', C30'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{C21, C22, C23, C24, C25, C26, C27, C28, C29, C30} sigma for 1-2: 0.02, 1-3:
0.04
as in
{C21', C22', C23', C24', C25', C26', C27', C28', C29', C30'}
7. Others
 Sof(C21')=Sof(H21')=Sof(C22')=Sof(C23')=Sof(H23')=Sof(C24')=Sof(H24')=
 Sof(C25')=Sof(H25')=Sof(C26')=Sof(H26')=Sof(C27')=Sof(H27')=Sof(C28')=
 Sof(H28')=Sof(C29')=Sof(C30')=1-FVAR(1)
 Sof(C21)=Sof(H21)=Sof(C22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=
 Sof(C30)=FVAR(1)
8.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C7(H7A,H7B), C13(H13A,H13B)
8.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4A), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C17(H17), C18(H18), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C21'(H21'), C23'(H23'), C24'(H24'), C25'(H25'),
 C26'(H26'), C27'(H27'), C28'(H28')
;
_shelx_res_checksum              7559
_shelx_hkl_checksum              90853
_shelx_fab_checksum              369
_olex2_submission_original_sample_id cwmwm15
_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 2.152
_oxdiff_exptl_absorpt_empirical_full_min 0.490