Amidino ligands obtained from the coupling of 1-methylcytosine and nitrile: a new method to incorporate biomolecules into luminescent Re(CO)3 complexes.
Gómez-Iglesias, Patricia; Martín-Alvarez, Jose Miguel; Miguel, Daniel; Villafañe, Fernando; Dalton transactions (Cambridge, England : 2003) 44 (2015) 17478–17481; doi:10.1039/c5dt03221k

data_7036564
_publ_section_title
;
 Amidino ligands obtained from the coupling of 1-methylcytosine and
 nitrile: a new method to incorporate biomolecules into luminescent
 Re(CO)3 complexes.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17478
_journal_page_last               17481
_journal_paper_doi               10.1039/c5dt03221k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C12 H13 N5 O4 Re, B F4'
_chemical_formula_sum            'C12 H13 B F4 N5 O4 Re'
_chemical_formula_weight         564.28
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-07-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-28 deposited with the CCDC.
2015-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4724(3)
_cell_length_b                   12.4285(2)
_cell_length_c                   20.5504(5)
_cell_measurement_reflns_used    3592
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9050
_cell_measurement_theta_min      2.9300
_cell_volume                     3696.41(13)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.813
_diffrn_measurement_details
;
  1 omega   26.00   82.00   1.0000  129.8050
omega____ theta____ kappa____ phi______ frames
    -        9.7850    0.0000  150.0000 56

  2 omega  -54.00  -11.00   1.0000  129.8050
omega____ theta____ kappa____ phi______ frames
    -        9.7850    0.0000  150.0000 43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0144937000
_diffrn_orient_matrix_UB_12      0.0061886000
_diffrn_orient_matrix_UB_13      -0.0327579000
_diffrn_orient_matrix_UB_21      -0.0337809000
_diffrn_orient_matrix_UB_22      -0.0378984000
_diffrn_orient_matrix_UB_23      -0.0100044000
_diffrn_orient_matrix_UB_31      -0.0324158000
_diffrn_orient_matrix_UB_32      0.0422357000
_diffrn_orient_matrix_UB_33      -0.0041991000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.813
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9372
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.813
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.003
_diffrn_reflns_theta_min         2.377
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.641
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_density_diffrn    2.028
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.2338
_exptl_crystal_size_mid          0.1065
_exptl_crystal_size_min          0.0522
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0323P)^2^+0.5902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2887
_reflns_number_total             3994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03221k2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7036563--7036564.cif.'
_cod_original_cell_volume        3696.40(14)
_cod_database_code               7036564
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'C12 H13 N5 O4 Re'
_reflns_odcompleteness_completeness 96.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(F2B)=Sof(F3B)=Sof(F4B)=1-FVAR(1)
 Sof(F3A)=Sof(F4A)=Sof(F2A)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), N3(H3), N4(H4)
3.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C22(H22A,H22B,H22C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              23863
_olex2_submission_special_instructions 'No special instructions were received'