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_7700770
_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         'C36 H33 N2 O3 P Re, F6 P'
_chemical_formula_sum            'C36 H33 F6 N2 O3 P2 Re'
_chemical_formula_weight         903.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-18
_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                68.440(3)
_cell_angle_beta                 70.666(4)
_cell_angle_gamma                64.490(4)
_cell_formula_units_Z            2
_cell_length_a                   11.6943(14)
_cell_length_b                   13.5357(15)
_cell_length_c                   13.6568(16)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.11
_cell_measurement_theta_min      3.05
_cell_volume                     1775.6(4)
_computing_cell_refinement       'Bruker Apex3 V.2017.3-0/SAINT V8.38A'
_computing_data_collection       'Bruker Apex3 V.2017.3-0'
_computing_data_reduction        'Bruker Apex3 V.2017.3-0/SAINT V8.38A'
_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_temperature      100
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker VENTURE CMOS area detector'
_diffrn_measurement_method       'shutterless omega and phi scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30421
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.195
_diffrn_reflns_theta_min         3.046
_diffrn_source                   'Incoatec IMuS microfocus Mo tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.582
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            'clear greenish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_description       plate
_exptl_crystal_F_000             892
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         5.400
_refine_diff_density_min         -3.029
_refine_diff_density_rms         0.334
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         10292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0813
_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^)+(0.0311P)^2^+57.6019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1896
_refine_ls_wR_factor_ref         0.2003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8716
_reflns_number_total             10292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02630d2.cif
_cod_data_source_block           s1
_cod_depositor_comments
'Adding full bibliography for 7700769--7700776.cif.'
_cod_database_code               7700770
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.534
_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. Rigid body (RIGU) restrains
 O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C10(H10), C24(H24), C23(H23), C34(H34), C35(H35), C33(H33), C15(H15),
 C3(H3), C32(H32), C36(H36), C12(H12), C22(H22), C30(H30), C13(H13), C4(H4),
 C26(H26), C7(H7), C5(H5), C29(H29), C14(H14), C20(H20), C27(H27), C21(H21),
 C28(H28)
3.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17C,H17A,H17B)
;
_shelx_res_checksum              31218
_olex2_submission_special_instructions 'No special instructions were received'