#------------------------------------------------------------------------------
#$Date: 2020-11-06 14:24:57 +0200 (Fri, 06 Nov 2020) $
#$Revision: 258872 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705323.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_7705323
loop_
_publ_author_name
'Lippi, Martina'
'Caputo, Josefina'
'Meneghetti, Fiorella'
'Castellano, Carlo'
'Martí-Rujas, Javier'
'Cametti, Massimo'
_publ_section_title
;
 Tuneable solvent adsorption and exchange by 1D bispidine-based Mn(II)
 coordination polymers via ligand design.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13420
_journal_page_last               13429
_journal_paper_doi               10.1039/d0dt02734k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C32 H34 Cl7 Mn0.5 N4 O6'
_chemical_formula_weight         846.25
_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   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2020-07-12 deposited with the CCDC.	2020-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                103.95(3)
_cell_angle_beta                 112.74(3)
_cell_angle_gamma                100.61(3)
_cell_formula_units_Z            2
_cell_length_a                   12.498(3)
_cell_length_b                   13.003(3)
_cell_length_c                   14.074(3)
_cell_measurement_reflns_used    4848
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.475
_cell_measurement_theta_min      2.528
_cell_volume                     1946.5(11)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0832
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10407
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        23.623
_diffrn_reflns_theta_max         23.623
_diffrn_reflns_theta_min         1.671
_exptl_absorpt_coefficient_mu    0.711
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       prism
_exptl_crystal_F_000             867
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.835
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         5616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0636
_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)+(0.0852P)²+3.6749P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.1810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3896
_reflns_number_total             5616
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02734k2.cif
_cod_data_source_block           L5TCM
_cod_depositor_comments
'Adding full bibliography for 7705323--7705327.cif.'
_cod_original_cell_volume        1946.4(8)
_cod_original_formula_sum        'C32 H34 Cl7 Mn0.50 N4 O6'
_cod_database_code               7705323
_shelx_shelxl_version_number     2017/1
_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.
;
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.979
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn 1.000000 0.000000 0.500000 0.0091(3) Uani 1 2 d S . P . .
Cl3 Cl 0.6322(2) -0.39336(16) 0.18922(17) 0.0514(6) Uani 1 1 d . . . . .
Cl7 Cl 1.1279(2) -0.15502(18) 0.20553(17) 0.0512(6) Uani 1 1 d . . . . .
Cl4 Cl 0.7251(2) -0.43414(17) 0.02556(18) 0.0515(6) Uani 1 1 d . . . . .
Cl2 Cl 0.5561(2) -0.30701(17) 0.00894(17) 0.0534(6) Uani 1 1 d . . . . .
Cl6 Cl 1.1076(2) 0.05523(15) 0.18305(18) 0.0481(6) Uani 1 1 d . . . . .
N1 N 1.2218(4) 0.5247(4) 0.4333(4) 0.0096(10) Uani 1 1 d . . . . .
Cl5 Cl 0.89773(18) -0.13941(17) 0.05702(16) 0.0494(5) Uani 1 1 d . . . . .
N3 N 1.0996(4) 0.8734(4) 0.4582(4) 0.0138(11) Uani 1 1 d . . . . .
O1 O 1.4499(4) 0.5243(3) 0.2942(3) 0.0186(9) Uani 1 1 d . . . . .
O2 O 1.4456(4) 0.3299(3) 0.3790(3) 0.0234(10) Uani 1 1 d . . . . .
N2 N 1.0864(4) 0.4417(4) 0.1947(4) 0.0104(10) Uani 1 1 d . . . . .
N4 N 1.0952(4) 0.1390(4) 0.4532(4) 0.0130(11) Uani 1 1 d . . . . .
O3 O 1.3134(4) 0.2465(3) 0.1982(3) 0.0241(10) Uani 1 1 d . . . . .
O4 O 1.4527(4) 0.7699(3) 0.3820(3) 0.0221(10) Uani 1 1 d . . . . .
C6 C 1.2808(5) 0.4039(4) 0.3010(4) 0.0093(12) Uani 1 1 d . . . . .
C5 C 1.2784(5) 0.4354(4) 0.4170(4) 0.0103(12) Uani 1 1 d . . . . .
H5 H 1.364644 0.463147 0.475800 0.012 Uiso 1 1 calc R U . . .
O5 O 1.3285(4) 0.7053(3) 0.1985(3) 0.0243(10) Uani 1 1 d . . . . .
C22 C 1.2114(5) 0.3325(4) 0.4295(4) 0.0085(12) Uani 1 1 d . . . . .
C4 C 1.2808(5) 0.6245(4) 0.4169(4) 0.0097(12) Uani 1 1 d . . . . .
H4 H 1.366763 0.657193 0.476312 0.012 Uiso 1 1 calc R U . . .
C20 C 1.2830(5) 0.8215(5) 0.4960(5) 0.0149(13) Uani 1 1 d . . . . .
H20 H 1.369590 0.843685 0.532119 0.018 Uiso 1 1 calc R U . . .
C29 C 1.3645(5) 0.7008(5) 0.3004(5) 0.0148(13) Uani 1 1 d . . . . .
C23 C 1.0833(5) 0.2883(4) 0.3792(4) 0.0122(13) Uani 1 1 d . . . . .
H23 H 1.033942 0.324014 0.337051 0.015 Uiso 1 1 calc R U . . .
C2 C 1.1593(5) 0.5454(4) 0.1957(5) 0.0119(12) Uani 1 1 d . . . . .
H2A H 1.113692 0.600129 0.193072 0.014 Uiso 1 1 calc R U . . .
H2B H 1.173357 0.529381 0.129760 0.014 Uiso 1 1 calc R U . . .
C21 C 1.2214(5) 0.8982(5) 0.5085(5) 0.0179(14) Uani 1 1 d . . . . .
H21 H 1.268227 0.972736 0.555531 0.021 Uiso 1 1 calc R U . . .
C27 C 1.3554(5) 0.3231(5) 0.2992(5) 0.0138(13) Uani 1 1 d . . . . .
C7 C 1.1535(5) 0.3596(4) 0.1975(4) 0.0108(12) Uani 1 1 d . . . . .
H7A H 1.165448 0.340811 0.130561 0.013 Uiso 1 1 calc R U . . .
H7B H 1.104255 0.290485 0.197278 0.013 Uiso 1 1 calc R U . . .
C8 C 0.9667(5) 0.3948(5) 0.0943(5) 0.0145(13) Uani 1 1 d . . . . .
H8A H 0.978187 0.355307 0.031198 0.017 Uiso 1 1 calc R U . . .
H8B H 0.935578 0.456510 0.078214 0.017 Uiso 1 1 calc R U . . .
C24 C 1.0296(5) 0.1924(5) 0.3917(5) 0.0132(13) Uani 1 1 d . . . . .
H24 H 0.943104 0.162532 0.355606 0.016 Uiso 1 1 calc R U . . .
C19 C 1.2152(5) 0.7110(4) 0.4292(4) 0.0121(13) Uani 1 1 d . . . . .
C17 C 1.0341(5) 0.7664(5) 0.3937(5) 0.0138(13) Uani 1 1 d . . . . .
H17 H 0.947664 0.747247 0.357594 0.017 Uiso 1 1 calc R U . . .
O6 O 0.6151(4) 0.1093(4) 0.1593(4) 0.0302(11) Uani 1 1 d . . . . .
C3 C 1.2851(5) 0.5962(4) 0.3013(5) 0.0124(13) Uani 1 1 d . . . . .
C1 C 1.3531(5) 0.5101(4) 0.2984(4) 0.0106(12) Uani 1 1 d . . . . .
C25 C 1.2186(5) 0.1844(5) 0.5023(5) 0.0160(14) Uani 1 1 d . . . . .
H25 H 1.266308 0.149135 0.546374 0.019 Uiso 1 1 calc R U . . .
C18 C 1.0876(5) 0.6830(4) 0.3779(4) 0.0118(13) Uani 1 1 d . . . . .
H18 H 1.038470 0.608387 0.333040 0.014 Uiso 1 1 calc R U . . .
C26 C 1.2795(5) 0.2786(5) 0.4923(5) 0.0146(13) Uani 1 1 d . . . . .
H26 H 1.366126 0.305834 0.527756 0.018 Uiso 1 1 calc R U . . .
C14 C 0.8547(5) 0.2010(5) 0.0749(5) 0.0185(14) Uani 1 1 d . . . . .
H14 H 0.899531 0.171039 0.040373 0.022 Uiso 1 1 calc R U . . .
C9 C 0.8737(5) 0.3150(5) 0.1079(4) 0.0147(13) Uani 1 1 d . . . . .
C33 C 1.2371(6) 0.5589(5) 0.5493(4) 0.0159(13) Uani 1 1 d . . . . .
H33A H 1.193135 0.495540 0.559989 0.019 Uiso 1 1 calc R U . . .
H33B H 1.204187 0.620797 0.562291 0.019 Uiso 1 1 calc R U . . .
H33C H 1.323976 0.582495 0.600901 0.019 Uiso 1 1 calc R U . . .
C13 C 0.7705(5) 0.1291(5) 0.0914(5) 0.0193(14) Uani 1 1 d . . . . .
H13 H 0.759606 0.051341 0.068749 0.023 Uiso 1 1 calc R U . . .
C10 C 0.8047(5) 0.3560(5) 0.1589(5) 0.0189(14) Uani 1 1 d . . . . .
H10 H 0.816841 0.433871 0.182938 0.023 Uiso 1 1 calc R U . . .
C12 C 0.7024(5) 0.1712(5) 0.1410(5) 0.0197(14) Uani 1 1 d . . . . .
C11 C 0.7202(5) 0.2864(5) 0.1749(5) 0.0211(14) Uani 1 1 d . . . . .
H11 H 0.674656 0.316320 0.208572 0.025 Uiso 1 1 calc R U . . .
C32 C 1.0345(6) -0.0707(5) 0.1871(6) 0.0282(16) Uani 1 1 d . . . . .
H32 H 1.011233 -0.055410 0.248351 0.034 Uiso 1 1 calc R U . . .
C28 C 1.3873(7) 0.1731(6) 0.1909(6) 0.0395(19) Uani 1 1 d . . . . .
H28A H 1.473283 0.217785 0.224668 0.047 Uiso 1 1 calc R U . . .
H28B H 1.360789 0.130942 0.113570 0.047 Uiso 1 1 calc R U . . .
H28C H 1.377475 0.121253 0.229360 0.047 Uiso 1 1 calc R U . . .
C31 C 0.6765(7) -0.3385(6) 0.1016(6) 0.0336(17) Uani 1 1 d . . . . .
H31 H 0.746291 -0.268254 0.147766 0.040 Uiso 1 1 calc R U . . .
Cl1 Cl 0.83536(12) -0.08381(11) 0.30667(11) 0.0152(4) Uani 1 1 d . . . . .
C30 C 1.4054(6) 0.7977(6) 0.1886(6) 0.0341(18) Uani 1 1 d . . . . .
H30A H 1.419126 0.867699 0.243757 0.041 Uiso 1 1 calc R U . . .
H30B H 1.364573 0.801683 0.115098 0.041 Uiso 1 1 calc R U . . .
H30C H 1.483871 0.785409 0.200231 0.041 Uiso 1 1 calc R U . . .
C34 C 0.5951(6) -0.0083(6) 0.1276(6) 0.0383(19) Uani 1 1 d . . . . .
H34A H 0.597237 -0.035079 0.057176 0.046 Uiso 1 1 calc R U . . .
H34B H 0.515340 -0.045915 0.120142 0.046 Uiso 1 1 calc R U . . .
H34C H 0.659190 -0.024374 0.183608 0.046 Uiso 1 1 calc R U . . .
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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
N3 Mn N3 180.0(2) 2_766 1_545 ?
N3 Mn N4 96.03(16) 2_766 2_756 ?
N3 Mn N4 83.97(16) 1_545 2_756 ?
N3 Mn N4 83.97(16) 2_766 . ?
N3 Mn N4 96.03(16) 1_545 . ?
N4 Mn N4 180.0 2_756 . ?
N3 Mn Cl1 90.65(12) 2_766 . ?
N3 Mn Cl1 89.35(12) 1_545 . ?
N4 Mn Cl1 90.37(12) 2_756 . ?
N4 Mn Cl1 89.63(12) . . ?
N3 Mn Cl1 89.35(12) 2_766 2_756 ?
N3 Mn Cl1 90.65(12) 1_545 2_756 ?
N4 Mn Cl1 89.63(12) 2_756 2_756 ?
N4 Mn Cl1 90.37(12) . 2_756 ?
Cl1 Mn Cl1 180.00(7) . 2_756 ?
C5 N1 C4 111.5(4) . . ?
C5 N1 C33 108.8(4) . . ?
C4 N1 C33 108.2(4) . . ?
C21 N3 C17 117.3(5) . . ?
C21 N3 Mn 122.2(4) . 1_565 ?
C17 N3 Mn 119.8(4) . 1_565 ?
C7 N2 C2 109.6(4) . . ?
C7 N2 C8 109.6(4) . . ?
C2 N2 C8 110.3(4) . . ?
C25 N4 C24 116.2(5) . . ?
C25 N4 Mn 121.6(3) . . ?
C24 N4 Mn 121.0(4) . . ?
C27 O3 C28 114.7(5) . . ?
C1 C6 C27 106.1(4) . . ?
C1 C6 C7 107.4(4) . . ?
C27 C6 C7 112.4(4) . . ?
C1 C6 C5 106.5(4) . . ?
C27 C6 C5 107.8(4) . . ?
C7 C6 C5 115.9(4) . . ?
N1 C5 C22 109.9(4) . . ?
N1 C5 C6 112.3(4) . . ?
C22 C5 C6 110.6(4) . . ?
C29 O5 C30 115.6(5) . . ?
C26 C22 C23 118.0(5) . . ?
C26 C22 C5 118.9(5) . . ?
C23 C22 C5 123.1(4) . . ?
N1 C4 C19 109.2(4) . . ?
N1 C4 C3 113.1(4) . . ?
C19 C4 C3 110.8(4) . . ?
C21 C20 C19 118.7(5) . . ?
O4 C29 O5 124.0(5) . . ?
O4 C29 C3 124.0(5) . . ?
O5 C29 C3 111.9(5) . . ?
C24 C23 C22 119.5(5) . . ?
N2 C2 C3 110.9(4) . . ?
N3 C21 C20 123.9(5) . . ?
O2 C27 O3 123.7(5) . . ?
O2 C27 C6 123.5(5) . . ?
O3 C27 C6 112.8(5) . . ?
N2 C7 C6 112.2(4) . . ?
N2 C8 C9 111.8(4) . . ?
N4 C24 C23 123.0(5) . . ?
C20 C19 C18 118.2(5) . . ?
C20 C19 C4 119.6(5) . . ?
C18 C19 C4 122.2(5) . . ?
N3 C17 C18 122.9(5) . . ?
C12 O6 C34 116.8(5) . . ?
C1 C3 C29 106.3(4) . . ?
C1 C3 C2 107.0(4) . . ?
C29 C3 C2 111.4(4) . . ?
C1 C3 C4 106.3(4) . . ?
C29 C3 C4 108.6(4) . . ?
C2 C3 C4 116.7(4) . . ?
O1 C1 C6 125.4(5) . . ?
O1 C1 C3 125.1(5) . . ?
C6 C1 C3 109.5(5) . . ?
N4 C25 C26 124.5(5) . . ?
C17 C18 C19 118.9(5) . . ?
C25 C26 C22 118.8(5) . . ?
C9 C14 C13 121.4(5) . . ?
C14 C9 C10 117.3(5) . . ?
C14 C9 C8 122.5(5) . . ?
C10 C9 C8 120.2(5) . . ?
C12 C13 C14 120.3(5) . . ?
C11 C10 C9 122.3(5) . . ?
O6 C12 C13 125.9(5) . . ?
O6 C12 C11 114.9(5) . . ?
C13 C12 C11 119.1(5) . . ?
C10 C11 C12 119.5(5) . . ?
Cl7 C32 Cl6 111.2(4) . . ?
Cl7 C32 Cl5 109.9(4) . . ?
Cl6 C32 Cl5 107.1(4) . . ?
Cl2 C31 Cl3 111.2(4) . . ?
Cl2 C31 Cl4 108.9(4) . . ?
Cl3 C31 Cl4 111.3(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn N3 2.336(4) 2_766 ?
Mn N3 2.336(4) 1_545 ?
Mn N4 2.345(5) 2_756 ?
Mn N4 2.345(5) . ?
Mn Cl1 2.4983(19) . ?
Mn Cl1 2.4983(19) 2_756 ?
Cl3 C31 1.773(7) . ?
Cl7 C32 1.734(7) . ?
Cl4 C31 1.788(7) . ?
Cl2 C31 1.761(7) . ?
Cl6 C32 1.747(7) . ?
N1 C5 1.483(7) . ?
N1 C4 1.484(7) . ?
N1 C33 1.509(7) . ?
Cl5 C32 1.817(7) . ?
N3 C21 1.341(7) . ?
N3 C17 1.352(7) . ?
O1 C1 1.216(6) . ?
O2 C27 1.215(7) . ?
N2 C7 1.473(6) . ?
N2 C2 1.475(7) . ?
N2 C8 1.490(7) . ?
N4 C25 1.359(7) . ?
N4 C24 1.363(7) . ?
O3 C27 1.355(7) . ?
O3 C28 1.458(7) . ?
O4 C29 1.225(7) . ?
C6 C1 1.522(8) . ?
C6 C27 1.529(8) . ?
C6 C7 1.565(8) . ?
C6 C5 1.598(8) . ?
C5 C22 1.529(7) . ?
O5 C29 1.347(7) . ?
O5 C30 1.464(7) . ?
C22 C26 1.390(7) . ?
C22 C23 1.409(8) . ?
C4 C19 1.524(7) . ?
C4 C3 1.604(8) . ?
C20 C21 1.386(8) . ?
C20 C19 1.397(8) . ?
C29 C3 1.535(8) . ?
C23 C24 1.388(8) . ?
C2 C3 1.567(8) . ?
C8 C9 1.512(8) . ?
C19 C18 1.403(8) . ?
C17 C18 1.393(8) . ?
O6 C12 1.378(7) . ?
O6 C34 1.429(8) . ?
C3 C1 1.527(8) . ?
C25 C26 1.386(8) . ?
C14 C9 1.386(8) . ?
C14 C13 1.403(8) . ?
C9 C10 1.417(8) . ?
C13 C12 1.400(8) . ?
C10 C11 1.384(8) . ?
C12 C11 1.403(9) . ?
