Synthesis and crystal structure of tricarbonylchlorido{1-[(pyridin-2-ylmethylidene)amino]adamantane}rhenium(I)
Jimenez, Jorge; Chakraborty, Indranil; Mascharak, Pradip; Acta Crystallographica Section E 72 (2016) 1276–1279; doi:10.1107/S205698901601255X

data_2241809
_publ_section_title
;
 Synthesis and crystal structure of
 tricarbonylchlorido{1-[(pyridin-2-ylmethylidene)amino]adamantane}rhenium(I)
;
_journal_coeditor_code           WM5310
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1276
_journal_page_last               1279
_journal_paper_doi               10.1107/S205698901601255X
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Re Cl (C16 H20 N2) (C O)3]'
_chemical_formula_moiety         'C19 H20 Cl N2 O3 Re'
_chemical_formula_sum            'C19 H20 Cl N2 O3 Re'
_chemical_formula_weight         546.02
_chemical_name_common
;
Tricarbonylchlorido{1-[(pyridin-2-ylmethylidene)amino]adamantane}rhenium(I)
;
_chemical_name_systematic
;
Tricarbonylchlorido{1-[(pyridin-2-ylmethylidene)amino]tricyclo[3.3.1.1^3,7^]\
decane}rhenium(I)
;
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.5090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.9550(6)
_cell_length_b                   21.7483(19)
_cell_length_c                   12.4482(11)
_cell_measurement_reflns_used    8126
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.10
_cell_measurement_theta_min      2.49
_cell_volume                     1877.1(3)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and CrystalMaker (Palmer, 2014)'
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20008
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.051
_diffrn_reflns_theta_min         2.490
_exptl_absorpt_coefficient_mu    6.637
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.4960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2012)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.546
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+0.9180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0501
_reflns_number_gt                4045
_reflns_number_total             4728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5310sup1.cif
_cod_data_source_block           I
_cod_database_code               2241809
_shelx_hkl_checksum              51226
_shelx_res_checksum              27251
_cod_database_fobs_code 2241809