Group 7 carbonyl complexes of a PNN-heteroscorpionate ligand
Valdivieso, Jorge P.; Erickson, Alexander N.; Gardinier, James R.; RSC Advances 14 (2024) 31502–31516; doi:10.1039/D4RA05287K

data_7249429
_publ_section_title
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 Group 7 carbonyl complexes of a PNN-heteroscorpionate ligand
;
_journal_issue                   43
_journal_name_full               'RSC Advances'
_journal_page_first              31502
_journal_page_last               31516
_journal_paper_doi               10.1039/D4RA05287K
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C30 H25 Br N4 O3 P Re'
_chemical_formula_sum            'C30 H25 Br N4 O3 P Re'
_chemical_formula_weight         786.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-17 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.9290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3314(2)
_cell_length_b                   13.5371(2)
_cell_length_c                   17.3610(3)
_cell_measurement_reflns_used    12870
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.6110
_cell_measurement_theta_min      3.6430
_cell_volume                     2824.62(8)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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   -117.00 -18.00   1.00    1.00    --  -42.46 -37.00  30.00   99
  2  \w    -81.00  27.00   1.00    1.00    --  -42.46  93.00 -67.00  108
  3  \w     23.00  98.00   1.00    1.00    --   42.46-125.00-150.00   75
  4  \w    101.00 178.00   1.00    1.12    --  100.00  93.00 -67.00   77
  5  \w     27.00 118.00   1.00    1.12    --  100.00-125.00 120.00   91
  6  \w     27.00 118.00   1.00    1.12    --  100.00-125.00  30.00   91
  7  \w     27.00 118.00   1.00    1.12    --  100.00-125.00-120.00   91
  8  \w     74.00 173.00   1.00    1.12    --  100.00  45.00   0.00   99
  9  \w     47.00 178.00   1.00    1.12    --  100.00  15.00 120.00  131
 10  \w     94.00 173.00   1.00    1.12    --  100.00 125.00 150.00   79
 11  \w   -119.00 -10.00   1.00    1.00    --  -42.46 -77.00 -30.00  109
 12  \w   -115.00 -14.00   1.00    1.00    --  -42.46 -57.00-120.00  101
 13  \w   -115.00 -14.00   1.00    1.00    --  -42.46 -57.00 150.00  101
 14  \w     94.00 140.00   1.00    1.12    --  100.00 125.00  30.00   46
 15  \w     71.00 172.00   1.00    1.12    --  100.00  61.00-180.00  101
 16  \w     72.00 176.00   1.00    1.12    --  100.00  30.00 -90.00  104
;
_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      -0.0817770000
_diffrn_orient_matrix_UB_12      -0.0761836000
_diffrn_orient_matrix_UB_13      -0.0468062000
_diffrn_orient_matrix_UB_21      -0.0290889000
_diffrn_orient_matrix_UB_22      0.0724356000
_diffrn_orient_matrix_UB_23      -0.0700478000
_diffrn_orient_matrix_UB_31      0.0942451000
_diffrn_orient_matrix_UB_32      -0.0436512000
_diffrn_orient_matrix_UB_33      -0.0345635000
_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  0.0475
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26425
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        70.648
_diffrn_reflns_theta_max         70.648
_diffrn_reflns_theta_min         4.007
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.932
_exptl_absorpt_correction_T_max  0.636
_exptl_absorpt_correction_T_min  0.135
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_description       prism
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.967
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         5354
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0340P)^2^+4.0831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4982
_reflns_number_total             5354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra05287k3.cif
_cod_data_source_block           1_gard25y
_cod_database_code               7249429
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C30H25BrN4O3PRe
_shelx_estimated_absorpt_t_max   0.354
_shelx_estimated_absorpt_t_min   0.127
_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
2. Others
 Fixed Sof: Br1A(0.8) Br1B(0.2) O2A(0.8) O2B(0.2) C9A(0.8) C9B(0.2)
3.a Ternary CH refined with riding coordinates:
 C7(H7)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C21(H21),
 C22(H22), C23(H23), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43),
  C45(H45), C46(H46)
3.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              64592
_shelx_hkl_checksum              40765
_olex2_submission_original_sample_id gard25y
_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 1.659
_oxdiff_exptl_absorpt_empirical_full_min 0.634