The crystal structure of fac-tricarbonyl(1,10-phenanthroline-κ2 N,N′)-(pyrazole-κN)rhenium(I)nitrate, C18H12O3N4Re
Ramoba, Lesetja V.; Alexander, Orbett T.; Visser, Hendrik G.; Manicum, Amanda-Lee E.; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1203–1205; doi:10.1515/ncrs-2020-0249

data_8105421
_publ_section_title
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 The crystal structure of fac-tricarbonyl(1,10-phenanthroline-\k2
 N,N&#x2032;)-(pyrazole-\kN)rhenium(I)nitrate, C18H12O3N4Re
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_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1203
_journal_page_last               1205
_journal_paper_doi               10.1515/ncrs-2020-0249
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C18 H12 N4 O3 Re, N O3'
_chemical_formula_sum            'C18 H12 N5 O6 Re'
_chemical_formula_weight         580.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                87.606(5)
_cell_angle_beta                 74.502(5)
_cell_angle_gamma                88.028(5)
_cell_formula_units_Z            2
_cell_length_a                   8.3476(15)
_cell_length_b                   9.5742(17)
_cell_length_c                   12.435(2)
_cell_measurement_reflns_used    4333
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3.954
_cell_volume                     956.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14935
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         3.954
_exptl_absorpt_coefficient_mu    6.400
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_description       Block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.508
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.246
_refine_diff_density_max         1.205
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4594
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0213
_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^)+(0.0222P)^2^+0.7667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0523
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4333
_reflns_number_total             4594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0249_suppl.cif
_cod_data_source_block           19pam1_0m
_cod_database_code               8105421
_shelx_estimated_absorpt_t_max   0.302
_shelx_estimated_absorpt_t_min   0.139
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N5-O4 \\sim N5-O5A \\sim N5-O6
 with sigma of 0.02
 O4A-O5 \\sim O5-O6 \\sim O6-O4A
 with sigma of 0.04
 N5-O4A \\sim N5-O5 \\sim N5-O6
 with sigma of 0.02
 O4-O5A \\sim O5A-O6 \\sim O6-O4
 with sigma of 0.04
3. Restrained planarity
 O6, N5, O4A, O5
 with sigma of 0.1
 O6, N5, O5A, O4
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O6 \\sim N5 \\sim O4A \\sim O5: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O6 \\sim N5 \\sim O5A \\sim O4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(O6) = Uanis(O4A) = Uanis(O4) = Uanis(O5A) = Uanis(O5)
5. Rigid body (RIGU) restrains
 O6, N5, O5, O4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.008
 O6, O5A, N5, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.008
6. Others
 Fixed Sof: O4(0.6) O5A(0.4) O4A(0.4) O5(0.6)
7.a Aromatic/amide H refined with riding coordinates:
 C4(H4A), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18)
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