#------------------------------------------------------------------------------
#$Date: 2019-11-24 06:21:31 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236936 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/99/4349908.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_4349908
loop_
_publ_author_name
'Wei, Yan-Li'
'Jing, Jing'
'Shi, Chao'
'Ye, Heng-Yun'
'Wang, Zhong-Xia'
'Zhang, Yi'
_publ_section_title
;
 High quantum yield and unusual photoluminescence behaviour in tetrahedral
 manganese(ii) based on hybrid compounds
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2615
_journal_paper_doi               10.1039/C8QI00793D
_journal_volume                  5
_journal_year                    2018
_chemical_formula_sum            'C12 H28 Cl4 Mn N2'
_chemical_formula_weight         397.10
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-07-18 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.99(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.526(3)
_cell_length_b                   12.021(2)
_cell_length_c                   13.124(3)
_cell_measurement_reflns_used    4493
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.482
_cell_measurement_theta_min      3.128
_cell_volume                     1961.5(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku, SCXmini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13209
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         3.128
_exptl_absorpt_coefficient_mu    1.209
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             828.0
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         4460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1157
_refine_ls_R_factor_gt           0.0645
_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)+(0.0313P)²+0.6112P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2908
_reflns_number_total             4460
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8qi00793d2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1961.6(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4349908
_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+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 0.24905(4) 0.08302(4) 0.20197(4) 0.05206(17) Uani 1 1 d . .
Cl2 Cl 0.44021(7) 0.09671(8) 0.24252(7) 0.0620(3) Uani 1 1 d . .
Cl3 Cl 0.21274(7) -0.03147(8) 0.05798(7) 0.0635(3) Uani 1 1 d . .
Cl4 Cl 0.18072(8) 0.26384(8) 0.16889(8) 0.0738(3) Uani 1 1 d . .
Cl5 Cl 0.17378(8) 0.02623(8) 0.34960(7) 0.0708(3) Uani 1 1 d . .
N2 N 0.4405(2) 0.2835(2) 0.4135(2) 0.0575(7) Uani 1 1 d . .
H2C H 0.4433 0.2258 0.3611 0.069 Uiso 1 1 calc R U
N1 N 0.9949(2) 0.2277(2) 0.3569(2) 0.0530(7) Uani 1 1 d . .
H1A H 1.0489 0.1755 0.3372 0.064 Uiso 1 1 calc R U
C4 C 0.3791(3) 0.2371(3) 0.4929(3) 0.0699(11) Uani 1 1 d . .
H4A H 0.3080 0.2153 0.4615 0.084 Uiso 1 1 calc R U
H4B H 0.3705 0.2938 0.5438 0.084 Uiso 1 1 calc R U
C2 C 0.9251(3) 0.2602(3) 0.2623(3) 0.0707(11) Uani 1 1 d . .
H2A H 0.9682 0.2960 0.2150 0.085 Uiso 1 1 calc R U
H2B H 0.8713 0.3129 0.2791 0.085 Uiso 1 1 calc R U
C7 C 0.4356(4) 0.1375(4) 0.5445(4) 0.0920(14) Uani 1 1 d . .
H7A H 0.4343 0.0767 0.4958 0.110 Uiso 1 1 calc R U
H7B H 0.3978 0.1135 0.6010 0.110 Uiso 1 1 calc R U
C5 C 0.9329(3) 0.1700(3) 0.4295(3) 0.0762(11) Uani 1 1 d . .
H5A H 0.8798 0.2206 0.4515 0.091 Uiso 1 1 calc R U
H5B H 0.9809 0.1478 0.4897 0.091 Uiso 1 1 calc R U
C12 C 0.5528(3) 0.3102(4) 0.4542(4) 0.0968(15) Uani 1 1 d . .
H12A H 0.5906 0.3374 0.3990 0.116 Uiso 1 1 calc R U
H12B H 0.5533 0.3687 0.5052 0.116 Uiso 1 1 calc R U
C6 C 1.0531(3) 0.3256(3) 0.4065(4) 0.0898(14) Uani 1 1 d . .
H6A H 1.0928 0.3618 0.3580 0.135 Uiso 1 1 calc R U
H6B H 1.0021 0.3768 0.4292 0.135 Uiso 1 1 calc R U
H6C H 1.1017 0.3011 0.4644 0.135 Uiso 1 1 calc R U
C13 C 0.3835(4) 0.3814(3) 0.3618(3) 0.0890(13) Uani 1 1 d . .
H13A H 0.4247 0.4102 0.3107 0.134 Uiso 1 1 calc R U
H13B H 0.3139 0.3588 0.3299 0.134 Uiso 1 1 calc R U
H13C H 0.3753 0.4381 0.4118 0.134 Uiso 1 1 calc R U
C9 C 0.8076(4) 0.0978(5) 0.2846(5) 0.1134(18) Uani 1 1 d . .
H9A H 0.7787 0.0298 0.2523 0.136 Uiso 1 1 calc R U
H9B H 0.7478 0.1434 0.3002 0.136 Uiso 1 1 calc R U
C10 C 0.8708(4) 0.1592(5) 0.2122(3) 0.1046(16) Uani 1 1 d . .
H10A H 0.8229 0.1819 0.1521 0.126 Uiso 1 1 calc R U
H10B H 0.9246 0.1100 0.1897 0.126 Uiso 1 1 calc R U
C14 C 0.8777(4) 0.0702(4) 0.3817(4) 0.1065(16) Uani 1 1 d . .
H14A H 0.8342 0.0368 0.4299 0.128 Uiso 1 1 calc R U
H14B H 0.9312 0.0160 0.3671 0.128 Uiso 1 1 calc R U
C15 C 0.6092(4) 0.2110(5) 0.5014(4) 0.1104(17) Uani 1 1 d . .
H15A H 0.6133 0.1544 0.4493 0.132 Uiso 1 1 calc R U
H15B H 0.6820 0.2311 0.5289 0.132 Uiso 1 1 calc R U
C16 C 0.5521(5) 0.1651(4) 0.5852(4) 0.1066(17) Uani 1 1 d . .
H16A H 0.5535 0.2191 0.6402 0.128 Uiso 1 1 calc R U
H16B H 0.5884 0.0984 0.6127 0.128 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'
Cl Cl 0.1484 0.1585 '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
Cl3 Mn1 Cl5 115.86(4)
Cl3 Mn1 Cl4 111.32(4)
Cl5 Mn1 Cl4 104.24(4)
Cl3 Mn1 Cl2 108.13(4)
Cl5 Mn1 Cl2 109.05(4)
Cl4 Mn1 Cl2 107.97(4)
C4 N2 C12 112.4(3)
C4 N2 C13 110.8(3)
C12 N2 C13 112.0(3)
C5 N1 C2 111.3(3)
C5 N1 C6 110.9(3)
C2 N1 C6 111.4(3)
N2 C4 C7 111.1(3)
N1 C2 C10 110.1(3)
C4 C7 C16 111.1(4)
N1 C5 C14 111.2(3)
C15 C12 N2 111.1(4)
C10 C9 C14 110.4(4)
C9 C10 C2 111.4(4)
C5 C14 C9 112.0(4)
C16 C15 C12 111.0(4)
C15 C16 C7 110.3(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mn1 Cl3 2.3374(10)
Mn1 Cl5 2.3567(11)
Mn1 Cl4 2.3570(11)
Mn1 Cl2 2.3945(11)
N2 C4 1.477(4)
N2 C12 1.478(5)
N2 C13 1.496(5)
N1 C5 1.474(4)
N1 C2 1.481(4)
N1 C6 1.492(4)
C4 C7 1.510(5)
C2 C10 1.503(6)
C7 C16 1.528(6)
C5 C14 1.485(6)
C12 C15 1.483(6)
C9 C10 1.503(7)
C9 C14 1.495(6)
C15 C16 1.488(7)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2C Cl2 0.98 2.20 3.174(3) 177.0 .
N1 H1A Cl5 0.98 2.37 3.309(3) 159.5 1_655
