#------------------------------------------------------------------------------
#$Date: 2016-09-10 02:35:40 +0300 (Sat, 10 Sep 2016) $
#$Revision: 186421 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/98/7039897.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_7039897
loop_
_publ_author_name
'Jimenez, Jorge'
'Chakraborty, Indranil'
'Carrington, Samantha J.'
'Mascharak, Pradip K.'
_publ_section_title
;
 Light-triggered CO delivery by a water-soluble and biocompatible
 manganese photoCORM.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13204
_journal_page_last               13213
_journal_paper_doi               10.1039/c6dt01358a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C20 H19 Br Mn N5 O3'
_chemical_formula_weight         512.25
_chemical_name_systematic        '[MnBr(CO)3(QTAm)]'
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-10 deposited with the CCDC.
2016-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                104.88(2)
_cell_angle_beta                 105.15(3)
_cell_angle_gamma                103.47(6)
_cell_formula_units_Z            2
_cell_length_a                   8.788(5)
_cell_length_b                   10.438(5)
_cell_length_c                   12.643(3)
_cell_measurement_reflns_used    2400
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      47.325
_cell_measurement_theta_min      5.076
_cell_volume                     1024.4(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7969
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        24.681
_diffrn_reflns_theta_max         24.681
_diffrn_reflns_theta_min         2.536
_exptl_absorpt_coefficient_mu    2.628
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       block
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.895
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0508
_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)+(0.1000P)²+0.7534P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1550
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2400
_reflns_number_total             3366
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt01358a2.cif
_cod_data_source_block           xsc1651_0m_a
_cod_depositor_comments
'Adding full bibliography for 7039895--7039897.cif.'
_cod_original_cell_volume        1024.3(8)
_cod_database_code               7039897
_shelx_shelxl_version_number     2014/7
_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.
;
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
Br1 Br 0.75388(7) 0.62800(6) 0.15178(5) 0.0513(3) Uani 1 1 d . .
Mn1 Mn 0.68140(8) 0.76743(7) 0.31430(6) 0.0296(2) Uani 1 1 d . .
N2 N 0.4350(4) 0.6813(4) 0.2012(3) 0.0255(8) Uani 1 1 d . .
N1 N 0.6048(5) 0.5796(4) 0.3466(4) 0.0322(9) Uani 1 1 d . .
O1 O 0.6241(6) 0.9255(5) 0.5181(4) 0.0624(12) Uani 1 1 d . .
O2 O 1.0430(5) 0.8624(4) 0.4391(5) 0.0730(15) Uani 1 1 d . .
O3 O 0.7916(6) 1.0267(5) 0.2647(4) 0.0716(14) Uani 1 1 d . .
N3 N 0.3216(6) 0.8499(5) -0.0260(4) 0.0460(12) Uani 1 1 d . .
N5 N 0.0642(5) 0.7272(5) -0.0032(4) 0.0443(11) Uani 1 1 d . .
N4 N 0.2460(5) 0.9546(4) 0.1419(4) 0.0419(11) Uani 1 1 d . .
C14 C 0.3375(5) 0.7472(5) 0.1314(4) 0.0275(10) Uani 1 1 d . .
C15 C 0.1546(6) 0.6540(5) 0.0640(5) 0.0362(12) Uani 1 1 d . .
H15A H 0.1511 0.5665 0.0114 0.043 Uiso 1 1 calc R U
H15B H 0.1011 0.6325 0.1183 0.043 Uiso 1 1 calc R U
C13 C 0.3739(6) 0.5531(5) 0.1890(4) 0.0342(12) Uani 1 1 d . .
H13 H 0.2709 0.4990 0.1325 0.041 Uiso 1 1 calc R U
C17 C 0.3357(6) 0.8843(5) 0.2117(5) 0.0347(12) Uani 1 1 d . .
H17A H 0.2814 0.8647 0.2661 0.042 Uiso 1 1 calc R U
H17B H 0.4490 0.9453 0.2560 0.042 Uiso 1 1 calc R U
C4 C 0.4648(6) 0.4922(5) 0.2630(4) 0.0328(11) Uani 1 1 d . .
C12 C 0.6876(6) 0.5321(5) 0.4289(5) 0.0362(12) Uani 1 1 d . .
C16 C 0.4147(6) 0.7776(6) 0.0405(5) 0.0369(12) Uani 1 1 d . .
H16A H 0.5303 0.8359 0.0794 0.044 Uiso 1 1 calc R U
H16B H 0.4112 0.6904 -0.0125 0.044 Uiso 1 1 calc R U
C18 C 0.3247(7) 0.9775(6) 0.0550(5) 0.0460(14) Uani 1 1 d . .
H18A H 0.2680 1.0269 0.0115 0.055 Uiso 1 1 calc R U
H18B H 0.4396 1.0368 0.0959 0.055 Uiso 1 1 calc R U
C2 C 0.9007(7) 0.8200(5) 0.3932(5) 0.0454(14) Uani 1 1 d . .
C1 C 0.6413(6) 0.8636(5) 0.4387(5) 0.0377(12) Uani 1 1 d . .
C3 C 0.7422(6) 0.9245(6) 0.2793(5) 0.0438(14) Uani 1 1 d . .
C7 C 0.6317(7) 0.3872(6) 0.4193(5) 0.0452(14) Uani 1 1 d . .
C20 C 0.1489(7) 0.7574(7) -0.0839(5) 0.0552(16) Uani 1 1 d . .
H20A H 0.0874 0.8004 -0.1317 0.066 Uiso 1 1 calc R U
H20B H 0.1475 0.6699 -0.1351 0.066 Uiso 1 1 calc R U
C19 C 0.0741(7) 0.8593(6) 0.0782(6) 0.0468(15) Uani 1 1 d . .
H19A H 0.0228 0.8394 0.1340 0.056 Uiso 1 1 calc R U
H19B H 0.0110 0.9060 0.0355 0.056 Uiso 1 1 calc R U
C8 C 0.7223(9) 0.3414(8) 0.5029(7) 0.0633(19) Uani 1 1 d . .
H8 H 0.6902 0.2470 0.4950 0.076 Uiso 1 1 calc R U
C6 C 0.4885(8) 0.2972(6) 0.3256(6) 0.0564(17) Uani 1 1 d . .
H6 H 0.4523 0.2022 0.3149 0.068 Uiso 1 1 calc R U
C5 C 0.4028(7) 0.3494(6) 0.2505(6) 0.0517(16) Uani 1 1 d . .
H5 H 0.3039 0.2915 0.1912 0.062 Uiso 1 1 calc R U
C9 C 0.8564(9) 0.4332(9) 0.5951(6) 0.070(2) Uani 1 1 d . .
H9 H 0.9143 0.4021 0.6506 0.084 Uiso 1 1 calc R U
C11 C 0.8251(7) 0.6242(6) 0.5267(5) 0.0506(15) Uani 1 1 d . .
H11 H 0.8605 0.7192 0.5373 0.061 Uiso 1 1 calc R U
C10 C 0.9063(9) 0.5738(8) 0.6060(6) 0.0644(18) Uani 1 1 d . .
H10 H 0.9982 0.6357 0.6694 0.077 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'
Br Br -0.2901 2.4595 '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'
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'
H H 0.0000 0.0000 '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_publ_flag
C2 Mn1 C1 92.5(3) y
C2 Mn1 C3 82.7(3) y
C1 Mn1 C3 90.7(3) y
C2 Mn1 N2 170.1(2) y
C1 Mn1 N2 97.1(2) y
C3 Mn1 N2 99.3(2) y
C2 Mn1 N1 98.9(2) y
C1 Mn1 N1 91.4(2) y
C3 Mn1 N1 177.3(2) y
N2 Mn1 N1 78.66(16) y
C2 Mn1 Br1 83.9(2) y
C1 Mn1 Br1 175.40(16) y
C3 Mn1 Br1 91.7(2) y
N2 Mn1 Br1 86.38(11) y
N1 Mn1 Br1 86.34(12) y
C13 N2 C14 120.0(4) ?
C13 N2 Mn1 111.8(3) ?
C14 N2 Mn1 128.0(3) ?
C4 N1 C12 118.9(4) ?
C4 N1 Mn1 110.8(3) ?
C12 N1 Mn1 129.6(3) ?
C18 N3 C20 108.9(5) ?
C18 N3 C16 108.6(4) ?
C20 N3 C16 107.5(4) ?
C19 N5 C20 108.9(5) ?
C19 N5 C15 108.3(4) ?
C20 N5 C15 107.8(4) ?
C19 N4 C17 107.6(4) ?
C19 N4 C18 108.0(4) ?
C17 N4 C18 109.2(4) ?
N2 C14 C17 109.6(4) ?
N2 C14 C16 110.1(4) ?
C17 C14 C16 109.6(4) ?
N2 C14 C15 113.0(4) ?
C17 C14 C15 107.5(4) ?
C16 C14 C15 107.0(4) ?
N5 C15 C14 110.0(4) ?
N5 C15 H15A 109.7 ?
C14 C15 H15A 109.7 ?
N5 C15 H15B 109.7 ?
C14 C15 H15B 109.7 ?
H15A C15 H15B 108.2 ?
N2 C13 C4 119.7(4) ?
N2 C13 H13 120.2 ?
C4 C13 H13 120.2 ?
N4 C17 C14 109.9(4) ?
N4 C17 H17A 109.7 ?
C14 C17 H17A 109.7 ?
N4 C17 H17B 109.7 ?
C14 C17 H17B 109.7 ?
H17A C17 H17B 108.2 ?
N1 C4 C5 122.6(5) ?
N1 C4 C13 115.9(4) ?
C5 C4 C13 121.4(4) ?
N1 C12 C11 121.2(5) ?
N1 C12 C7 120.7(5) ?
C11 C12 C7 118.1(5) ?
N3 C16 C14 110.1(4) ?
N3 C16 H16A 109.6 ?
C14 C16 H16A 109.6 ?
N3 C16 H16B 109.6 ?
C14 C16 H16B 109.6 ?
H16A C16 H16B 108.2 ?
N3 C18 N4 113.9(4) ?
N3 C18 H18A 108.8 ?
N4 C18 H18A 108.8 ?
N3 C18 H18B 108.8 ?
N4 C18 H18B 108.8 ?
H18A C18 H18B 107.7 ?
O2 C2 Mn1 174.0(5) ?
O1 C1 Mn1 176.9(5) ?
O3 C3 Mn1 174.6(5) ?
C6 C7 C8 122.8(6) ?
C6 C7 C12 118.1(5) ?
C8 C7 C12 119.2(6) ?
N5 C20 N3 113.7(5) ?
N5 C20 H20A 108.8 ?
N3 C20 H20A 108.8 ?
N5 C20 H20B 108.8 ?
N3 C20 H20B 108.8 ?
H20A C20 H20B 107.7 ?
N5 C19 N4 113.3(4) ?
N5 C19 H19A 108.9 ?
N4 C19 H19A 108.9 ?
N5 C19 H19B 108.9 ?
N4 C19 H19B 108.9 ?
H19A C19 H19B 107.7 ?
C9 C8 C7 120.9(6) ?
C9 C8 H8 119.6 ?
C7 C8 H8 119.6 ?
C5 C6 C7 119.8(5) ?
C5 C6 H6 120.1 ?
C7 C6 H6 120.1 ?
C6 C5 C4 119.7(5) ?
C6 C5 H5 120.2 ?
C4 C5 H5 120.2 ?
C8 C9 C10 119.6(6) ?
C8 C9 H9 120.2 ?
C10 C9 H9 120.2 ?
C10 C11 C12 119.9(6) ?
C10 C11 H11 120.1 ?
C12 C11 H11 120.1 ?
C11 C10 C9 122.2(7) ?
C11 C10 H10 118.9 ?
C9 C10 H10 118.9 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Br1 Mn1 2.5152(12) y
Mn1 C2 1.797(5) y
Mn1 C1 1.802(6) y
Mn1 C3 1.805(6) y
Mn1 N2 2.087(4) y
Mn1 N1 2.098(4) y
N2 C13 1.272(6) ?
N2 C14 1.475(6) ?
N1 C4 1.329(6) ?
N1 C12 1.377(6) ?
O1 C1 1.113(7) ?
O2 C2 1.152(6) ?
O3 C3 1.135(7) ?
N3 C18 1.446(8) ?
N3 C20 1.464(7) ?
N3 C16 1.483(7) ?
N5 C19 1.462(8) ?
N5 C20 1.465(8) ?
N5 C15 1.484(6) ?
N4 C19 1.474(7) ?
N4 C17 1.476(7) ?
N4 C18 1.482(7) ?
C14 C17 1.533(7) ?
C14 C16 1.542(7) ?
C14 C15 1.544(6) ?
C15 H15A 0.9700 ?
C15 H15B 0.9700 ?
C13 C4 1.438(7) ?
C13 H13 0.9300 ?
C17 H17A 0.9700 ?
C17 H17B 0.9700 ?
C4 C5 1.413(7) ?
C12 C11 1.407(8) ?
C12 C7 1.440(7) ?
C16 H16A 0.9700 ?
C16 H16B 0.9700 ?
C18 H18A 0.9700 ?
C18 H18B 0.9700 ?
C7 C6 1.403(8) ?
C7 C8 1.406(8) ?
C20 H20A 0.9700 ?
C20 H20B 0.9700 ?
C19 H19A 0.9700 ?
C19 H19B 0.9700 ?
C8 C9 1.359(10) ?
C8 H8 0.9300 ?
C6 C5 1.360(8) ?
C6 H6 0.9300 ?
C5 H5 0.9300 ?
C9 C10 1.389(10) ?
C9 H9 0.9300 ?
C11 C10 1.364(8) ?
C11 H11 0.9300 ?
C10 H10 0.9300 ?
