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_7036563
_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         'C10 H10 Br N4 O4 Re, C3 H6 O'
_chemical_formula_sum            'C13 H16 Br N4 O5 Re'
_chemical_formula_weight         574.41
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-28
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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_audit_update_record
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2015-07-28 deposited with the CCDC.
2015-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.660(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1440(3)
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_cell_length_c                   11.5351(3)
_cell_measurement_reflns_used    3832
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0130
_cell_measurement_theta_min      2.5760
_cell_volume                     1805.90(10)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_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    'ShelXS (Sheldrick, 2008)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.801
_diffrn_measurement_details
;
  1 omega  -66.00   17.00   1.0000   25.7450
omega____ theta____ kappa____ phi______ frames
    -       -7.9100  -57.0000  120.0000 83

  2 omega  -51.00   19.00   1.0000   25.7450
omega____ theta____ kappa____ phi______ frames
    -        9.7850  -37.0000  -90.0000 70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
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_diffrn_orient_matrix_UB_11      0.0059429000
_diffrn_orient_matrix_UB_12      0.0449753000
_diffrn_orient_matrix_UB_13      0.0024897000
_diffrn_orient_matrix_UB_21      -0.0383119000
_diffrn_orient_matrix_UB_22      0.0019748000
_diffrn_orient_matrix_UB_23      -0.0683435000
_diffrn_orient_matrix_UB_31      -0.0597724000
_diffrn_orient_matrix_UB_32      0.0032043000
_diffrn_orient_matrix_UB_33      0.0072559000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.801
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7516
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.801
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.984
_diffrn_reflns_theta_min         2.363
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.971
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_colour            yellow
_exptl_crystal_density_diffrn    2.113
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.1988
_exptl_crystal_size_mid          0.1082
_exptl_crystal_size_min          0.0768
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.002
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0133P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3220
_reflns_number_total             3849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03221k2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7036563--7036564.cif.'
_cod_original_cell_volume        1805.90(9)
_cod_database_code               7036563
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'C12 H12 N5 O4 Re1'
_reflns_odcompleteness_completeness 96.48
_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.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N3(H3), C12(H12), C13(H13)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C22(H22A,H22B,H22C), C93(H93A,H93B,H93C), C92(H92A,H92B,
 H92C)
;
_shelx_res_checksum              10051
_olex2_submission_special_instructions 'No special instructions were received'