Steric influence of salicylaldehyde-based Schiff base ligands on the formation of trans-[Re(PR<sub>3</sub>)<sub>2</sub>(Schiff base)]<sup>+</sup> complexes.
Baumeister, Jakob E.; Mitchell, Andrew W.; Kelley, Steven P.; Barnes, Charles L.; Jurisson, Silvia S.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 12943–12955; doi:10.1039/c9dt02630d

data_7700772
_publ_section_title
;
 Steric influence of salicylaldehyde-based Schiff base ligands on the
 formation of trans-[Re(PR<sub>3</sub>)<sub>2</sub>(Schiff
 base)]<sup>+</sup> complexes.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12943
_journal_page_last               12955
_journal_paper_doi               10.1039/c9dt02630d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C46 H48 N2 O2 P2 Re, F6 P'
_chemical_formula_sum            'C48.33 H57.33 F6 N2 O4.33 P3 Re'
_chemical_formula_weight         1128.73
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-07-27
_audit_creation_method
; 
Olex2 1.2 
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) 
;
_audit_update_record
;
2019-07-27 deposited with the CCDC.    2019-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 130.2840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.450(4)
_cell_length_b                   10.1296(9)
_cell_length_c                   30.348(3)
_cell_measurement_reflns_used    9005
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.43
_cell_volume                     9954.9(16)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            220929
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.289
_diffrn_reflns_theta_min         2.435
_diffrn_source                   'Sealed Source Mo with TRIUMPH optics'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.605
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.0621 before and 0.0483 after correction. 
The Ratio of minimum to maximum transmission is 0.8049. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       Needle
_exptl_crystal_F_000             4560
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol/Water'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         12348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0196
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+19.8539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10909
_reflns_number_total             12348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02630d2.cif
_cod_data_source_block           jeb288_sq
_cod_depositor_comments
'Adding full bibliography for 7700769--7700776.cif.'
_cod_original_cell_volume        9955.0(15)
_cod_database_code               7700772
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.463
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2.a Secondary CH2 refined with riding coordinates: 
 C8(H8A,H8B), C19(H19A,H19B), C33(H33A,H33B) 
2.b Aromatic/amide H refined with riding coordinates: 
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C12(H12), C13(H13), 
 C14(H14), C15(H15), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), 
  C29(H29), C30(H30), C31(H31), C32(H32), C36(H36), C37(H37), C38(H38), 
 C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46) 
2.c Idealised Me refined as rotating group: 
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C34(H34A,H34B, 
 H34C) 
;
_shelx_res_checksum              77700
_shelx_fab_checksum              19673
_olex2_submission_special_instructions 'No special instructions were received'