Bond length of perchlorate at different temperatures: X-ray and neutron comparison
Olmstead, Marilyn M.; Acta Crystallographica Section C 76 (2020) –; doi:10.1107/S2053229620000388

data_2021953
_publ_section_title
;
 Bond length of perchlorate at different temperatures: X-ray and neutron
 comparison
;
_journal_coeditor_code           OP3001
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229620000388
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Mn (C20 H20 N5 O1) (N O)] Cl O4, 2C2 H3 N'
_chemical_formula_moiety         'C20 H20 Mn N6 O2, Cl O4, 2(C2 H3 N)'
_chemical_formula_sum            'C24 H26 Cl Mn N8 O6'
_chemical_formula_weight         612.92
_chemical_name_common            '[Mn(PaPy3)(NO)](ClO4).2(CH3CN)'
_chemical_name_systematic
'(<i>N</i>-{2-[Bis(pyridin-2-ylmethyl)amino]ethyl}pyridine-2-carboxamidato)(nitric oxide)manganese perchlorate acetonitrile disolvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 98.3222(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3188(4)
_cell_length_b                   14.1117(6)
_cell_length_c                   11.6994(5)
_cell_measurement_reflns_used    6558
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.27
_cell_volume                     1358.96(10)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
SMART (Bruker, 2003)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
<b>[Program(s) used to create the graphics?]</b>
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15578
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_min         2.276
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2016)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.255
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2534 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.015(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         6155
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+0.1568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0717
_reflns_number_gt                5730
_reflns_number_total             6155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            op3001sup1.cif
_cod_data_source_block           mn1486
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2021953
_shelx_estimated_absorpt_t_min   0.827
_shelx_estimated_absorpt_t_max   0.951
_shelx_hkl_checksum              44761
_shelx_res_checksum              3683
_cod_database_fobs_code 2021953