Tuning the reaction pathways of phenanthroline-Schiff bases: routes to novel phenanthroline ligands.
Ahmed, Muhib; Rooney, Denise; McCann, Malachy; Casey, Jamie; O'Shea, Katie; Twamley, Brendan; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15283–15289; doi:10.1039/c9dt03084k

data_7701309
_publ_section_title
;
 Tuning the reaction pathways of phenanthroline-Schiff bases: routes to
 novel phenanthroline ligands.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15283
_journal_page_last               15289
_journal_paper_doi               10.1039/c9dt03084k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C27 H17 Br N3 O6 Re'
_chemical_formula_sum            'C27 H17 Br N3 O6 Re'
_chemical_formula_weight         745.54
_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             2019-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-18 deposited with the CCDC.    2019-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                83.1740(16)
_cell_angle_beta                 74.5305(15)
_cell_angle_gamma                78.6214(16)
_cell_formula_units_Z            2
_cell_length_a                   8.5421(3)
_cell_length_b                   10.0776(4)
_cell_length_c                   15.2032(6)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.622
_cell_measurement_theta_min      3.0235
_cell_volume                     1233.50(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX 3 (Bruker, 2017) '
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 Kappa Duo'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       APEX2
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17848
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.537
_diffrn_reflns_theta_min         3.023
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    11.963
_exptl_absorpt_correction_T_max  0.9042
_exptl_absorpt_correction_T_min  0.4049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.352
_refine_diff_density_min         -1.822
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         4591
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0699P)^2^+1.2791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4369
_reflns_number_total             4591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03084k2.cif
_cod_data_source_block           1c
_cod_depositor_comments
'Adding full bibliography for 7701308--7701310.cif.'
_cod_database_code               7701309
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.715
_shelx_estimated_absorpt_t_min   0.305
_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. Restrained distances
 C25-C10
 1.48 with sigma of 0.01
 Re1-C33 = Re1-C33A
 1.95 with sigma of 0.01
 O34-C33 = O34A-C33A
 1.15 with sigma of 0.01
 Re1-Br1A \\sim Re1-Br1
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Br1 \\sim Br1A \\sim O34 \\sim O34A \\sim C33 \\sim C33A: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: Br1(0.95) Br1A(0.05) O34(0.95) O34A(0.05) C33(0.95) C33A(0.05)
5.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C13(H13), C14(H14), C20(H20), C21(H21), C22(H22),
 C23(H23), C24(H24)
5.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              45614
_olex2_exptl_crystal_mounting_method 'mounted in oil on a MiTeGen microloop'
_olex2_submission_original_sample_id JCRe1
_olex2_submission_special_instructions 'No special instructions were received'