#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:36:15 +0100 (vie 08 de nov de 2019) $
#$Revision: 224526 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/08/7700826.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7700826
loop_
_publ_author_name
'Mączka, Mirosław'
'Gągor, Anna'
'Ptak, Maciej'
'Stefańska, Dagmara'
'Macalik, Lucyna'
'Pikul, Adam'
'Sieradzki, Adam'
_publ_section_title
;
 Structural, phonon, magnetic and optical properties of novel
 perovskite-like frameworks of TriBuMe[M(dca)₃] (TriBuMe =
 tributylmethylammonium; dca = dicyanamide; M = Mn²⁺,
 Fe²⁺, Co²⁺, Ni²⁺).
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13006
_journal_page_last               13016
_journal_paper_doi               10.1039/c9dt02924a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C38 H60 Mn2 N20'
_chemical_formula_weight         906.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-07-11 deposited with the CCDC.    2019-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8900(18)
_cell_length_b                   17.0382(18)
_cell_length_c                   13.0657(15)
_cell_measurement_reflns_used    1578
_cell_measurement_temperature    375.00(10)
_cell_measurement_theta_max      23.6180
_cell_measurement_theta_min      3.5870
_cell_volume                     2424.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      375.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7967
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.678
_diffrn_reflns_theta_max         25.678
_diffrn_reflns_theta_min         2.713
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       prism
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2384
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.0826
_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/[σ²(Fo²)+(0.1700P)²+0.1600P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2659
_refine_ls_wR_factor_ref         0.3134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1332
_reflns_number_total             2384
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02924a2.cif
_cod_data_source_block           PhaseI
_cod_depositor_comments
'Adding full bibliography for 7700826--7700827.cif.'
_cod_database_code               7700826
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.962
_oxdiff_exptl_absorpt_empirical_full_max 1.062
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Mn1 Mn 0.500000 0.500000 0.500000 0.0557(5) Uani 1 2 d S . P
N1 N 0.5139(4) 0.3791(2) 0.5634(3) 0.0868(16) Uani 1 1 d . . .
N2A N 0.583(3) 0.250000 0.6297(12) 0.065(7) Uiso 0.41(4) 2 d S . P
N2B N 0.521(2) 0.250000 0.6469(12) 0.078(5) Uiso 0.59(4) 2 d S . P
N3 N 0.6003(4) 0.5456(3) 0.6368(4) 0.0894(15) Uani 1 1 d . . .
N4A N 0.6719(10) 0.5845(7) 0.8043(7) 0.0815(19) Uiso 0.555(16) 1 d . . P
N4B N 0.6395(13) 0.5543(9) 0.8245(9) 0.0815(19) Uiso 0.445(16) 1 d . . P
N5 N 0.8254(5) 0.5187(3) 0.9159(4) 0.0922(15) Uani 1 1 d . . .
C1 C 0.5282(5) 0.3175(3) 0.5942(4) 0.0763(15) Uani 1 1 d . . .
C2 C 0.6320(5) 0.5545(3) 0.7182(4) 0.0785(15) Uani 1 1 d . . .
C3 C 0.7512(6) 0.5407(3) 0.8639(4) 0.0823(15) Uani 1 1 d . . .
N6 N 0.6255(9) 0.250000 0.0060(8) 0.162(5) Uani 1 2 d DS T P
C4 C 0.7492(13) 0.2055(13) 0.000(2) 0.218(14) Uani 0.5 1 d D . P
C5 C 0.6123(19) 0.250000 0.1244(9) 0.286(13) Uani 1 2 d DS T P
C6 C 0.635(2) 0.250000 0.2339(11) 0.56(5) Uani 1 2 d DS T P
C7 C 0.554(2) 0.250000 0.3220(17) 0.291(18) Uani 1 2 d DS T P
C8 C 0.674(2) 0.250000 0.369(2) 0.261(12) Uani 1 2 d DS T P
C9 C 0.536(2) 0.1823(12) -0.0229(17) 0.227(10) Uiso 0.64(2) 1 d D . P
C10 C 0.6190(19) 0.1793(16) -0.068(3) 0.227(10) Uiso 0.36(2) 1 d D . P
C11 C 0.5201(15) 0.1338(11) -0.1130(15) 0.311(12) Uani 1 1 d D . .
C12 C 0.4264(15) 0.0781(9) -0.1435(13) 0.250(6) Uani 1 1 d D U .
C13A C 0.302(3) 0.049(5) -0.149(7) 0.221(7) Uiso 0.176(19) 1 d D . P
C13B C 0.3239(16) 0.1230(11) -0.1820(12) 0.221(7) Uiso 0.824(19) 1 d D . P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N5 Mn1 N5 180.0 6_557 2_664
N5 Mn1 N3 91.56(17) 6_557 5_666
N5 Mn1 N3 88.44(17) 2_664 5_666
N5 Mn1 N3 88.44(17) 6_557 .
N5 Mn1 N3 91.56(17) 2_664 .
N3 Mn1 N3 180.0 5_666 .
N5 Mn1 N1 89.57(18) 6_557 5_666
N5 Mn1 N1 90.43(18) 2_664 5_666
N3 Mn1 N1 89.49(17) 5_666 5_666
N3 Mn1 N1 90.52(17) . 5_666
N5 Mn1 N1 90.43(18) 6_557 .
N5 Mn1 N1 89.57(18) 2_664 .
N3 Mn1 N1 90.51(17) 5_666 .
N3 Mn1 N1 89.48(17) . .
N1 Mn1 N1 180.0(2) 5_666 .
C1 N1 Mn1 175.9(5) . .
C1 N2A C1 113.6(15) 7_565 .
C1 N2B C1 117.8(13) 7_565 .
C2 N3 Mn1 161.9(5) . .
C2 N4A C3 118.7(8) . .
C3 N4B C2 115.8(10) . .
C3 N5 Mn1 165.1(5) . 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N5 2.219(5) 6_557
Mn1 N5 2.219(5) 2_664
Mn1 N3 2.234(5) 5_666
Mn1 N3 2.234(5) .
Mn1 N1 2.226(4) 5_666
Mn1 N1 2.226(4) .
