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_7700773
_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         'C44 H44 N2 O2 P2 Re, Cl'
_chemical_formula_sum            'C46 H52 Cl N2 O4 P2 Re'
_chemical_formula_weight         980.48
_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
_audit_creation_date             2019-01-16
_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                100.0420(10)
_cell_angle_beta                 91.4370(10)
_cell_angle_gamma                106.1440(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5691(6)
_cell_length_b                   12.4434(8)
_cell_length_c                   17.0828(10)
_cell_measurement_reflns_used    9810
_cell_measurement_temperature    223
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      2.27
_cell_volume                     2118.6(2)
_computing_cell_refinement       'Bruker Apex3 V.2016.9-0/SAINT V8.37A'
_computing_data_collection       'Bruker Apex3 V.2016.9-0'
_computing_data_reduction        'Bruker Apex3 V.2016.9-0/SAINT V8.37A'
_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      223
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.0487
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            74295
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.663
_diffrn_reflns_theta_min         1.735
_diffrn_source                   'Sealed Source Mo with TRIUMPH optics'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.052
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.917
_refine_diff_density_min         -1.428
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         14260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0354P)^2^+0.9305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11623
_reflns_number_total             14260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02630d2.cif
_cod_data_source_block           s1_sq
_cod_depositor_comments
'Adding full bibliography for 7700769--7700776.cif.'
_cod_database_code               7700773
_shelx_shelxl_version_number     2017/1
_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), C43(H43A,H43B), C29(H29A,H29B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C15(H15), C10(H10), C32(H32), C18(H18), C38(H38), C35(H35), C28(H28),
 C42(H42), C24(H24), C2(H2), C36(H36), C39(H39), C12(H12), C22(H22), C13(H13),
 C3(H3), C27(H27), C4(H4), C25(H25), C40(H40), C34(H34), C5(H5), C14(H14),
 C19(H19), C33(H33), C26(H26), C41(H41), C20(H20), C21(H21)
2.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              16243
_shelx_fab_checksum              60646
_olex2_submission_special_instructions 'No special instructions were received'