Carbon Nitride as a Ligand: Edge-Site Coordination of ReCl(CO)3-fragments to g-C3N4
Coulson, Ben; Issacs, Mark; Lari, Leonardo; Douthwaite, Richard E. E.; Duhme-klair, Anne-Kathrin; Chemical Communications  (2019) –; doi:10.1039/C9CC02197C

data_7123586
_publ_section_title
;
 Carbon Nitride as a Ligand: Edge-Site Coordination of ReCl(CO)3-fragments
 to g-C3N4
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02197C
_journal_year                    2019
_chemical_formula_moiety         'C13 H11 Cl N3 O3 Re, 0.59(H2 O)'
_chemical_formula_sum            'C13 H12.18 Cl N3 O3.59 Re'
_chemical_formula_weight         489.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-15 deposited with the CCDC.    2019-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.0420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.6764(2)
_cell_length_b                   12.05740(10)
_cell_length_c                   20.0284(2)
_cell_measurement_reflns_used    8829
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      31.7720
_cell_measurement_theta_min      3.9410
_cell_volume                     3049.38(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.930
_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    -47.00  70.00   1.00   50.00    --   25.54 -19.00  90.00  117
  2  \w    -20.00  67.00   1.00   50.00    --   25.54 -99.00 -90.00   87
  3  \w    -97.00 -35.00   1.00   50.00    --  -25.86 147.00  47.00   62
  4  \w      4.00  94.00   1.00   50.00    --   25.54  57.00  90.00   90
  5  \w     35.00 101.00   1.00   50.00    --   25.54 178.00 120.00   66
  6  \w      4.00  29.00   1.00   50.00    --   25.54  57.00 -60.00   25
  7  \w      4.00  94.00   1.00   50.00    --   25.54  57.00-150.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0196795000
_diffrn_orient_matrix_UB_12      0.0539530000
_diffrn_orient_matrix_UB_13      -0.0055502000
_diffrn_orient_matrix_UB_21      -0.0499355000
_diffrn_orient_matrix_UB_22      0.0228577000
_diffrn_orient_matrix_UB_23      0.0058344000
_diffrn_orient_matrix_UB_31      0.0166079000
_diffrn_orient_matrix_UB_32      0.0048251000
_diffrn_orient_matrix_UB_33      0.0346392000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19729
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.088
_diffrn_reflns_theta_min         3.530
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.162
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.132
_exptl_crystal_description       plate
_exptl_crystal_F_000             1855
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.516
_refine_diff_density_min         -2.003
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0136P)^2^+14.4651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4563
_reflns_number_total             4946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02197c2.cif
_cod_data_source_block           ReCl(CO)3DMNA
_cod_database_code               7123586
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C13 H12.2 N3 O3.6 Cl Re'
_chemical_oxdiff_usercomment     'Ben Coulson BC269'
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.368
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(O5)=Sof(H5A)=Sof(H5B)=FVAR(1)
 Sof(O4)=Sof(H4A)=Sof(H4B)=FVAR(2)
3.a Free rotating group:
 O4(H4A,H4B), O5(H5A,H5B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C4(H4)
3.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C)
;
_olex2_date_sample_data_collection 2017-08-08
_olex2_exptl_crystal_mounting_method 'oil on 75 micrometre micromount'
_olex2_submission_original_sample_id BC269
_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 1.527
_oxdiff_exptl_absorpt_empirical_full_min 0.786