Crystal structures and Hirshfeld surface analysis of [κ^2^-<i>P</i>,<i>N</i>-{(C~6~H~5~)~2~(C~5~H~5~N)P}Re(CO)~3~Br]·2CHCl~3~ and the product of its reaction with piperidine, [<i>P</i>-{(C~6~H~5~)~2~(C~5~H~5~N)P}(C~5~H~11~N)Re(CO)~3~Br]
Palominos, Franco; Muñoz, Carolina; Oyarzun, Poldie; Saldías, Marianela; Vega, Andrés; Acta Crystallographica Section E 75 (2019) 1005–1010; doi:10.1107/S2056989019008089

data_2242983
_publ_section_title
;
 Crystal structures and Hirshfeld surface analysis of
 [\k^2^-<i>P</i>,<i>N</i>-{(C~6~H~5~)~2~(C~5~H~5~N)P}Re(CO)~3~Br]&#x00B7;2CHCl~3~
 and the product of its reaction with piperidine,
 [<i>P</i>-{(C~6~H~5~)~2~(C~5~H~5~N)P}(C~5~H~11~N)Re(CO)~3~Br]
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1005
_journal_page_last               1010
_journal_paper_doi               10.1107/S2056989019008089
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'[Re Br (C5 H11 N) (C17 H14 N P) (C O)3], [+ solvent]'
_chemical_formula_moiety         'C25 H25 Br N2 O3 P Re'
_chemical_formula_sum            'C25 H25 Br N2 O3 P Re'
_chemical_formula_weight         698.55
_chemical_name_systematic
Bromidotricarbonyl[diphenyl(pyridin-2-yl)phosphane-\k<i>P</i>](piperidine-\k<i>N</i>)rhenium(I)
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                82.956(2)
_cell_angle_beta                 82.047(2)
_cell_angle_gamma                69.765(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1384(17)
_cell_length_b                   9.8348(18)
_cell_length_c                   15.671(3)
_cell_measurement_reflns_used    4721
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.82
_cell_measurement_theta_min      2.39
_cell_volume                     1304.5(4)
_computing_cell_refinement
;
SMART (Bruker, 2012)
;
_computing_data_collection
;
SMART (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015), PLATON (Spek, 2009)
and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10214
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.214
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    6.278
_exptl_absorpt_correction_T_max  0.8581
_exptl_absorpt_correction_T_min  0.5602
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_description       stick
_exptl_crystal_F_000             676.0
_exptl_crystal_size_max          0.067
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.962
_refine_diff_density_min         -1.791
_refine_ls_extinction_coef       0.00125(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         5113
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0416
_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^)+9.4699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0820
_reflns_number_gt                4493
_reflns_number_total             5113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nk2249sup1.cif
_cod_data_source_block           II
_cod_database_code               2242983
_shelx_estimated_absorpt_t_min   0.678
_shelx_estimated_absorpt_t_max   0.834
_shelx_hkl_checksum              70280
_shelx_res_checksum              70370
_shelx_fab_checksum              20536
_cod_database_fobs_code 2242983