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#$Date: 2018-01-06 03:42:11 +0200 (Sat, 06 Jan 2018) $
#$Revision: 204785 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/28/4002875.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_4002875
loop_
_publ_author_name
'Wong, Man Kwong'
'Liu, Fangzhou'
'Kam, Chun Sing'
'Leung, Tik Lun'
'Tam, Ho Won'
'Djurišić, Aleksandra B.'
'Popović, Jasminka'
'Li, Hangkong'
'Shih, Kaimin'
'Low, Kam-Hung'
'Chan, Wai Kin'
'Chen, Wei'
'He, Zhubing'
'Ng, Annie'
'Surya, Charles'
_publ_section_title
;
 Synthesis of Lead-Free Perovskite Films by Combinatorial Evaporation:
 Fast Processes for Screening Different Precursor Combinations
;
_journal_issue                   23
_journal_name_full               'Chemistry of Materials'
_journal_page_first              9946
_journal_paper_doi               10.1021/acs.chemmater.7b03293
_journal_volume                  29
_journal_year                    2017
_chemical_formula_moiety         'Br4 Pd, 2(C3 H10 N)'
_chemical_formula_sum            'C6 H20 Br4 N2 Pd'
_chemical_formula_weight         546.28
_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-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.089(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7344(15)
_cell_length_b                   8.5264(11)
_cell_length_c                   7.5155(9)
_cell_measurement_reflns_used    174
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.8
_cell_volume                     735.27(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2013)'
_computing_data_collection       'APEX3 v2015.5-2 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 VENTURE FIXED-CHI PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7780
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.592
_diffrn_reflns_theta_min         2.976
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    12.099
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.2506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Sheldrick, 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.467
_exptl_crystal_description       plate
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.034
_refine_diff_density_max         1.414
_refine_diff_density_min         -1.997
_refine_diff_density_rms         0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         2238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0407
_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)+(0.0360P)²+1.0642P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1823
_reflns_number_total             2238
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm7b03293_si_001.cif
_cod_data_source_block           mo_CHEM0433
_cod_depositor_comments
'Adding full bibliography for 4002873--4002875.cif.'
_cod_database_code               4002875
_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.
;
_shelx_estimated_absorpt_t_min   0.099
_shelx_estimated_absorpt_t_max   0.684
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
_atom_site_refinement_flags_occupancy
Pd1 Pd 0.5000 0.5000 0.5000 0.00916(12) Uani 1 2 d S . P
Br1 Br 0.29110(4) 0.55308(5) 0.39700(6) 0.01541(13) Uani 1 1 d . . .
Br2 Br 0.54277(4) 0.70536(5) 0.29722(6) 0.01319(13) Uani 1 1 d . . .
N1 N 0.3293(4) -0.0505(5) 0.4507(6) 0.0159(9) Uani 1 1 d . . .
H1A H 0.3717 0.0214 0.4028 0.024 Uiso 1 1 calc R U .
H1B H 0.3535 -0.1488 0.4290 0.024 Uiso 1 1 calc R U .
H1C H 0.3396 -0.0351 0.5728 0.024 Uiso 1 1 calc R U .
C1 C 0.2037(5) -0.0328(6) 0.3647(8) 0.0211(11) Uani 1 1 d . . .
H1D H 0.1577 -0.1113 0.4165 0.025 Uiso 1 1 calc R U .
H1E H 0.1922 -0.0526 0.2323 0.025 Uiso 1 1 calc R U .
C2 C 0.1607(5) 0.1283(6) 0.3952(8) 0.0232(12) Uani 1 1 d . . .
H2A H 0.2098 0.2071 0.3499 0.028 Uiso 1 1 calc R U .
H2B H 0.1679 0.1458 0.5273 0.028 Uiso 1 1 calc R U .
C3 C 0.0351(6) 0.1498(8) 0.2988(9) 0.0395(16) Uani 1 1 d . . .
H3A H 0.0278 0.1320 0.1680 0.059 Uiso 1 1 calc R U .
H3B H 0.0100 0.2568 0.3189 0.059 Uiso 1 1 calc R U .
H3C H -0.0140 0.0747 0.3468 0.059 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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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
Br2 Pd1 Br2 179.999(15) . 3_666
Br2 Pd1 Br1 90.392(17) . 3_666
Br2 Pd1 Br1 89.609(17) 3_666 3_666
Br2 Pd1 Br1 89.608(17) . .
Br2 Pd1 Br1 90.391(17) 3_666 .
Br1 Pd1 Br1 180.0 3_666 .
C1 N1 H1A 109.5 . .
C1 N1 H1B 109.5 . .
H1A N1 H1B 109.5 . .
C1 N1 H1C 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
N1 C1 C2 111.2(4) . .
N1 C1 H1D 109.4 . .
C2 C1 H1D 109.4 . .
N1 C1 H1E 109.4 . .
C2 C1 H1E 109.4 . .
H1D C1 H1E 108.0 . .
C1 C2 C3 111.3(5) . .
C1 C2 H2A 109.4 . .
C3 C2 H2A 109.4 . .
C1 C2 H2B 109.4 . .
C3 C2 H2B 109.4 . .
H2A C2 H2B 108.0 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 Br2 2.4414(5) .
Pd1 Br2 2.4414(5) 3_666
Pd1 Br1 2.4532(6) 3_666
Pd1 Br1 2.4532(6) .
N1 C1 1.489(7) .
N1 H1A 0.9100 .
N1 H1B 0.9100 .
N1 H1C 0.9100 .
C1 C2 1.497(7) .
C1 H1D 0.9900 .
C1 H1E 0.9900 .
C2 C3 1.512(8) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
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
N1 C1 C2 C3 176.7(5)
