#------------------------------------------------------------------------------
#$Date: 2019-11-23 19:00:58 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234554 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/51/7125143.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_7125143
loop_
_publ_author_name
'Coogan, M. P.'
'Platts, J. A.'
_publ_section_title
;
 Blue rhenium tricarbonyl DPPZ complexes - low energy charge-transfer
 absorption at tissue-penetrating wavelengths.
;
_journal_issue                   84
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12498
_journal_page_last               12501
_journal_paper_doi               10.1039/c6cc07125b
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C10.5 H5 Br0.5 Mn0.5 N2 O1.5'
_chemical_formula_sum            'C10.5 H6 Br0.5 Mn0.5 N2 O2'
_chemical_formula_weight         259.60
_chemical_name_common            MnBrCO3dppz
_chemical_name_systematic        MnBrCO3dppz
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-08
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2016-08-22 deposited with the CCDC.
2016-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.067(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.4756(5)
_cell_length_b                   12.4761(3)
_cell_length_c                   7.29758(16)
_cell_measurement_reflns_used    5605
_cell_measurement_temperature    292.78(10)
_cell_measurement_theta_max      77.0350
_cell_measurement_theta_min      3.7780
_cell_volume                     2121.11(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.78(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2303
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00 -18.00   1.00    1.00    --  -38.50 -38.00-150.00   92
  2  ω    -64.00  30.00   1.00    1.00    --  -38.50  57.00   0.00   94
  3  ω     17.00 111.00   1.00    1.00    --   42.14  57.00-150.00   94
  4  ω     23.00  96.00   1.00    1.00    --   42.14-125.00 -90.00   73
  5  ω    100.00 178.00   1.00    1.64    --  111.00 111.00 -30.00   78
  6  ω     71.00 178.00   1.00    1.64    --  111.00  15.00 -60.00  107
  7  ω    100.00 178.00   1.00    1.64    --  111.00 111.00  60.00   78
  8  ω    100.00 178.00   1.00    1.64    --  111.00 111.00 150.00   78
  9  ω     99.00 178.00   1.00    1.64    --  111.00  88.00 -74.00   79
 10  ω     40.00 141.00   1.00    1.64    --  111.00 -77.00-180.00  101
 11  ω     31.00 109.00   1.00    1.64    --  111.00 -94.00  60.00   78
 12  ω     41.00 133.00   1.00    1.64    --  111.00 -45.00 150.00   92
 13  ω     85.00 178.00   1.00    1.64    --  111.00  61.00 150.00   93
 14  ω    -29.00  63.00   1.00    1.00    --   42.14 -38.00  60.00   92
 15  ω     17.00 111.00   1.00    1.00    --   42.14  57.00  30.00   94
 16  ω     17.00 111.00   1.00    1.00    --   42.14  57.00 120.00   94
 17  ω     81.00 176.00   1.00    1.64    --  111.00  77.00  90.00   95
 18  ω     85.00 178.00   1.00    1.64    --  111.00  61.00-150.00   93
 19  ω     71.00 178.00   1.00    1.64    --  111.00  15.00  60.00  107
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0099969000
_diffrn_orient_matrix_UB_12      0.0753962000
_diffrn_orient_matrix_UB_13      0.1601252000
_diffrn_orient_matrix_UB_21      0.0421614000
_diffrn_orient_matrix_UB_22      0.0813919000
_diffrn_orient_matrix_UB_23      -0.0667219000
_diffrn_orient_matrix_UB_31      -0.0499666000
_diffrn_orient_matrix_UB_32      0.0541268000
_diffrn_orient_matrix_UB_33      -0.1231991000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11582
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.309
_diffrn_reflns_theta_min         3.795
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.582
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0352P)²+2.2005P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2142
_reflns_number_total             2340
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6cc07125b2.cif
_cod_data_source_block           mc143
_cod_original_formula_sum        'C10.50 H6 Br0.50 Mn0.50 N2 O2'
_cod_database_code               7125143
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C21 H10 N4O3 Br1 Mn1'
_chemical_oxdiff_usercomment     'Mn dppz br 100K'
_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.
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C10(H10), C16(H16), C17(H17)
;
_olex2_date_sample_data_collection 2016-06-08
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.520
_oxdiff_exptl_absorpt_empirical_full_min 0.788
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Br1 Br 0.73841(2) 0.5000 1.10981(4) 0.02280(10) Uani 1 2 d S T P
Mn2 Mn 0.79583(2) 0.5000 0.83710(6) 0.01902(12) Uani 1 2 d S T P
O3 O 0.86318(9) 0.5000 0.5233(3) 0.0270(4) Uani 1 2 d S T P
O5 O 0.87488(7) 0.66597(14) 1.0096(2) 0.0367(4) Uani 1 1 d . . .
N7 N 0.73578(7) 0.39514(13) 0.7123(2) 0.0187(3) Uani 1 1 d . . .
N14 N 0.55203(7) 0.38620(15) 0.3391(2) 0.0243(4) Uani 1 1 d . . .
C12 C 0.73562(9) 0.28814(16) 0.7271(3) 0.0211(4) Uani 1 1 d . . .
H12 H 0.7660 0.2547 0.7990 0.025 Uiso 1 1 calc R . .
C8 C 0.69074(8) 0.44200(15) 0.6087(3) 0.0187(4) Uani 1 1 d . . .
C4 C 0.83714(12) 0.5000 0.6412(4) 0.0211(6) Uani 1 2 d S T P
C9 C 0.64506(8) 0.38435(16) 0.5159(3) 0.0202(4) Uani 1 1 d . . .
C13 C 0.59645(8) 0.44279(16) 0.4182(3) 0.0209(4) Uani 1 1 d . . .
C11 C 0.69149(9) 0.22496(17) 0.6382(3) 0.0235(4) Uani 1 1 d . . .
H11 H 0.6928 0.1508 0.6513 0.028 Uiso 1 1 calc R . .
C15 C 0.50637(9) 0.44278(18) 0.2584(3) 0.0254(4) Uani 1 1 d . . .
C10 C 0.64614(9) 0.27234(17) 0.5312(3) 0.0226(4) Uani 1 1 d . . .
H10 H 0.6168 0.2310 0.4702 0.027 Uiso 1 1 calc R . .
C6 C 0.84368(9) 0.60235(18) 0.9455(3) 0.0259(4) Uani 1 1 d . . .
C16 C 0.45745(9) 0.3870(2) 0.1734(3) 0.0305(5) Uani 1 1 d . . .
H16 H 0.4570 0.3125 0.1725 0.037 Uiso 1 1 calc R . .
C17 C 0.41100(9) 0.4433(2) 0.0929(3) 0.0335(5) Uani 1 1 d . . .
H17 H 0.3790 0.4065 0.0374 0.040 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
N7 Mn2 Br1 86.89(5) . .
N7 Mn2 Br1 86.89(5) 6_565 .
N7 Mn2 N7 79.20(9) . 6_565
C4 Mn2 Br1 179.97(9) . .
C4 Mn2 N7 93.13(8) . .
C4 Mn2 N7 93.13(8) . 6_565
C6 Mn2 Br1 91.04(7) . .
C6 Mn2 Br1 91.04(7) 6_565 .
C6 Mn2 N7 174.58(8) . .
C6 Mn2 N7 95.70(8) . 6_565
C6 Mn2 N7 95.70(8) 6_565 .
C6 Mn2 N7 174.58(8) 6_565 6_565
C6 Mn2 C4 88.94(9) . .
C6 Mn2 C4 88.94(9) 6_565 .
C6 Mn2 C6 89.34(14) 6_565 .
C12 N7 Mn2 127.47(14) . .
C12 N7 C8 117.72(17) . .
C8 N7 Mn2 114.77(13) . .
C13 N14 C15 116.59(19) . .
N7 C12 H12 118.8 . .
N7 C12 C11 122.32(19) . .
C11 C12 H12 118.8 . .
N7 C8 C8 115.57(11) . 6_565
N7 C8 C9 123.30(18) . .
C9 C8 C8 121.03(12) . 6_565
O3 C4 Mn2 178.9(3) . .
C8 C9 C13 119.10(18) . .
C8 C9 C10 118.03(18) . .
C10 C9 C13 122.73(18) . .
N14 C13 C9 118.00(19) . .
N14 C13 C13 122.04(12) . 6_565
C13 C13 C9 119.87(11) 6_565 .
C12 C11 H11 120.0 . .
C10 C11 C12 119.98(19) . .
C10 C11 H11 120.0 . .
N14 C15 C15 121.37(12) . 6_565
N14 C15 C16 119.3(2) . .
C16 C15 C15 119.37(14) . 6_565
C9 C10 H10 120.7 . .
C11 C10 C9 118.64(19) . .
C11 C10 H10 120.7 . .
O5 C6 Mn2 177.9(2) . .
C15 C16 H16 120.1 . .
C17 C16 C15 119.7(2) . .
C17 C16 H16 120.1 . .
C16 C17 C17 120.89(15) . 6_565
C16 C17 H17 119.6 . .
C17 C17 H17 119.6 6_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Mn2 2.5373(5) .
Mn2 N7 2.0524(17) .
Mn2 N7 2.0524(16) 6_565
Mn2 C4 1.824(3) .
Mn2 C6 1.816(2) 6_565
Mn2 C6 1.816(2) .
O3 C4 1.115(4) .
O5 C6 1.141(3) .
N7 C12 1.339(3) .
N7 C8 1.354(3) .
N14 C13 1.331(3) .
N14 C15 1.356(3) .
C12 H12 0.9300 .
C12 C11 1.396(3) .
C8 C8 1.447(4) 6_565
C8 C9 1.395(3) .
C9 C13 1.464(3) .
C9 C10 1.402(3) .
C13 C13 1.428(4) 6_565
C11 H11 0.9300 .
C11 C10 1.374(3) .
C15 C15 1.428(5) 6_565
C15 C16 1.419(3) .
C10 H10 0.9300 .
C16 H16 0.9300 .
C16 C17 1.367(3) .
C17 C17 1.416(5) 6_565
C17 H17 0.9300 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Mn2 N7 C12 C11 178.57(14) . .
Mn2 N7 C8 C8 -2.58(13) . 6_565
Mn2 N7 C8 C9 -178.79(14) . .
N7 C12 C11 C10 -0.1(3) . .
N7 C8 C9 C13 175.73(16) . .
N7 C8 C9 C10 0.0(3) . .
N14 C15 C16 C17 179.51(18) . .
C12 N7 C8 C8 175.42(13) . 6_565
C12 N7 C8 C9 -0.8(3) . .
C12 C11 C10 C9 -0.8(3) . .
C8 N7 C12 C11 0.9(3) . .
C8 C8 C9 C13 -0.3(2) 6_565 .
C8 C8 C9 C10 -176.06(12) 6_565 .
C8 C9 C13 N14 -176.46(17) . .
C8 C9 C13 C13 0.3(2) . 6_565
C8 C9 C10 C11 0.8(3) . .
C13 N14 C15 C15 0.2(2) . 6_565
C13 N14 C15 C16 -179.36(17) . .
C13 C9 C10 C11 -174.79(17) . .
C15 N14 C13 C9 176.48(16) . .
C15 N14 C13 C13 -0.2(2) . 6_565
C15 C15 C16 C17 -0.1(2) 6_565 .
C15 C16 C17 C17 0.1(2) . 6_565
C10 C9 C13 N14 -0.9(3) . .
C10 C9 C13 C13 175.85(14) . 6_565
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 0.000 0.500 -0.618 192.6 46.8
2 0.500 0.000 -0.194 192.6 46.8
