Tricarbonylchlorido(6',7'-dihydro-5'<i>H</i>-spiro[cyclopentane-1,6'-dipyrido[3,2-<i>d</i>:2',3'-<i>f</i>][1,3]diazepine]-κ^2^<i>N</i>^1^,<i>N</i>^11^)rhenium(I)
Clegg, Oliver R.; Harding, Lindsay P.; Miller, John W.; Rice, Craig R.; Acta Crystallographica Section E 69 (2013) m526–; doi:10.1107/S1600536813023076

data_2238648
_publ_section_title
;
 Tricarbonylchlorido(6',7'-dihydro-5'<i>H</i>-spiro[cyclopentane-1,6'-dipyrido[3,2-<i>d</i>:2',3'-<i>f</i>][1,3]diazepine]-\k^2^<i>N</i>^1^,<i>N</i>^11^)rhenium(I)
;
_journal_coeditor_code           LH5644
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m526
_journal_paper_doi               10.1107/S1600536813023076
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Re Cl (C15 H16 N4) (C O)3]'
_chemical_formula_moiety         'C18 H16 Cl N4 O3 Re'
_chemical_formula_sum            'C18 H16 Cl N4 O3 Re'
_chemical_formula_weight         558.00
_chemical_name_systematic
Tricarbonylchlorido(6',7'-dihydro-5'<i>H</i>-spiro[cyclopentane-1,6'-dipyrido[3,2-<i>d</i>:2',3'-<i>f</i>][1,3]diazepine]-\k^2^<i>N</i>^1^,<i>N</i>^11^)rhenium(I)
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.1162(5)
_cell_length_b                   11.9638(5)
_cell_length_c                   24.9181(9)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      39.3170
_cell_measurement_theta_min      2.8980
_cell_volume                     3612.0(2)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'OLEX2 (Dolomanov <i>et al.</i>, 2009)'
_computing_publication_material  'OLEX2 (Dolomanov <i>et al.</i>, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            45382
_diffrn_reflns_theta_full        39.39
_diffrn_reflns_theta_max         39.39
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    6.904
_exptl_absorpt_correction_T_max  0.34
_exptl_absorpt_correction_T_min  0.16
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.052
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.276
_refine_diff_density_min         -5.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         10757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0093P)^2^+8.4209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0749
_reflns_number_gt                7941
_reflns_number_total             10757
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5644.cif
_cod_data_source_block           I
_cod_database_code               2238648