#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:26:29 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180039 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/33/7033325.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_7033325
loop_
_publ_author_name
'Agarwal, Jay'
'Stanton Iii, Charles J.'
'Shaw, Travis W.'
'Vandezande, Jonathon E.'
'Majetich, George F.'
'Bocarsly, Andrew B.'
'Schaefer Iii, Henry F.'
_publ_section_title
;
 Exploring the effect of axial ligand substitution (X = Br, NCS, CN) on
 the photodecomposition and electrochemical activity of [MnX(N-C)(CO)3]
 complexes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2122
_journal_page_last               2131
_journal_paper_doi               10.1039/c4dt03079f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C13 H11 Br Mn N3 O3'
_chemical_formula_weight         392.10
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-06-14 deposited with the CCDC.
2014-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.8260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3770(9)
_cell_length_b                   10.7747(7)
_cell_length_c                   9.6613(6)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.56
_cell_measurement_theta_min      2.38
_cell_volume                     1459.27(16)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'OMEGA SCAN'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23397
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.031
_diffrn_reflns_theta_min         2.384
_exptl_absorpt_coefficient_mu    3.655
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.3754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         5066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0302
_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)+(0.0447P)²+1.0927P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4427
_reflns_number_total             5066
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt03079f2.cif
_cod_data_source_block           j1
_cod_depositor_comments
'Adding full bibliography for 7033325--7033329.cif.'
_cod_database_code               7033325
#BEGIN Tags that were not found in dictionaries:
_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   0.309
_shelx_estimated_absorpt_t_max   0.811
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Mn1 Mn 0.79843(2) -0.05411(2) 0.50328(3) 0.01312(7) Uani 1 1 d . .
Br1 Br 0.65885(2) -0.02752(2) 0.29151(2) 0.01606(6) Uani 1 1 d . .
N1 N 0.64825(12) -0.01496(14) 0.69394(17) 0.0150(3) Uani 1 1 d . .
N2 N 0.71620(11) 0.14591(13) 0.62996(16) 0.0134(3) Uani 1 1 d . .
N3 N 0.82528(11) 0.13476(14) 0.49115(16) 0.0139(3) Uani 1 1 d . .
C1 C 0.71306(13) 0.01869(16) 0.61954(19) 0.0138(3) Uani 1 1 d . .
C2 C 0.61067(14) 0.08885(17) 0.7488(2) 0.0174(3) Uani 1 1 d . .
H2A H 0.5636 0.0880 0.8040 0.021 Uiso 1 1 calc R U
C3 C 0.65324(13) 0.19042(17) 0.7096(2) 0.0166(3) Uani 1 1 d . .
H3A H 0.6426 0.2745 0.7314 0.020 Uiso 1 1 calc R U
C4 C 0.77756(13) 0.21027(16) 0.56137(19) 0.0135(3) Uani 1 1 d . .
C5 C 0.78723(14) 0.33881(16) 0.5654(2) 0.0164(3) Uani 1 1 d . .
H5A H 0.7513 0.3888 0.6156 0.020 Uiso 1 1 calc R U
C6 C 0.85095(14) 0.39142(18) 0.4940(2) 0.0188(3) Uani 1 1 d . .
H6A H 0.8599 0.4788 0.4948 0.023 Uiso 1 1 calc R U
C7 C 0.90189(14) 0.31507(18) 0.4208(2) 0.0188(3) Uani 1 1 d . .
H7A H 0.9460 0.3494 0.3713 0.023 Uiso 1 1 calc R U
C8 C 0.88681(14) 0.18842(17) 0.4217(2) 0.0166(3) Uani 1 1 d . .
H8A H 0.9213 0.1366 0.3712 0.020 Uiso 1 1 calc R U
C9 C 0.61500(15) -0.14234(17) 0.7065(2) 0.0181(3) Uani 1 1 d . .
H9A H 0.5901 -0.1497 0.7938 0.022 Uiso 1 1 calc R U
H9B H 0.6693 -0.2004 0.7147 0.022 Uiso 1 1 calc R U
C10 C 0.53698(15) -0.17773(19) 0.5783(2) 0.0214(4) Uani 1 1 d . .
H10A H 0.5161 -0.2630 0.5895 0.032 Uiso 1 1 calc R U
H10B H 0.5619 -0.1719 0.4920 0.032 Uiso 1 1 calc R U
H10C H 0.4828 -0.1211 0.5709 0.032 Uiso 1 1 calc R U
C11 C 0.89274(14) -0.07459(16) 0.6667(2) 0.0180(4) Uani 1 1 d . .
O1 O 0.94521(12) -0.08887(15) 0.76260(18) 0.0257(3) Uani 1 1 d . .
C12 C 0.76772(14) -0.21592(17) 0.5124(2) 0.0171(3) Uani 1 1 d . .
O2 O 0.75252(12) -0.32033(13) 0.51610(16) 0.0240(3) Uani 1 1 d . .
C13 C 0.87469(14) -0.09782(17) 0.3812(2) 0.0179(3) Uani 1 1 d . .
O3 O 0.92189(12) -0.12794(15) 0.30604(18) 0.0274(3) Uani 1 1 d . .
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'
Br Br -0.2901 2.4595 '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
C12 Mn1 C13 88.35(8)
C12 Mn1 C11 89.08(8)
C13 Mn1 C11 95.05(8)
C12 Mn1 C1 99.44(8)
C13 Mn1 C1 171.02(8)
C11 Mn1 C1 89.57(7)
C12 Mn1 N3 176.61(8)
C13 Mn1 N3 94.01(7)
C11 Mn1 N3 93.14(7)
C1 Mn1 N3 78.02(7)
C12 Mn1 Br1 89.44(6)
C13 Mn1 Br1 89.39(6)
C11 Mn1 Br1 175.28(6)
C1 Mn1 Br1 86.25(5)
N3 Mn1 Br1 88.14(4)
C1 N1 C2 111.03(16)
C1 N1 C9 124.95(16)
C2 N1 C9 123.83(16)
C1 N2 C4 118.26(15)
C1 N2 C3 111.60(15)
C4 N2 C3 130.13(15)
C4 N3 C8 117.12(15)
C4 N3 Mn1 116.29(12)
C8 N3 Mn1 126.59(12)
N1 C1 N2 104.17(15)
N1 C1 Mn1 141.09(13)
N2 C1 Mn1 114.73(13)
C3 C2 N1 107.74(16)
C2 C3 N2 105.45(15)
N3 C4 C5 123.97(17)
N3 C4 N2 112.70(15)
C5 C4 N2 123.33(16)
C6 C5 C4 117.79(17)
C5 C6 C7 119.44(17)
C8 C7 C6 118.60(18)
N3 C8 C7 123.08(17)
N1 C9 C10 111.18(15)
O1 C11 Mn1 177.64(18)
O2 C12 Mn1 176.42(18)
O3 C13 Mn1 178.37(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mn1 C12 1.8055(19)
Mn1 C13 1.8407(19)
Mn1 C11 1.852(2)
Mn1 C1 1.9989(18)
Mn1 N3 2.0795(15)
Mn1 Br1 2.5441(4)
N1 C1 1.347(2)
N1 C2 1.397(2)
N1 C9 1.467(2)
N2 C1 1.374(2)
N2 C4 1.399(2)
N2 C3 1.396(2)
N3 C4 1.341(2)
N3 C8 1.353(2)
C2 C3 1.349(3)
C4 C5 1.392(2)
C5 C6 1.385(3)
C6 C7 1.394(3)
C7 C8 1.382(3)
C9 C10 1.524(3)
C11 O1 1.068(3)
C12 O2 1.148(2)
C13 O3 1.146(2)
